# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 #============================================================================== _audit_creation_method 'form.cif (version 2.0)' _publ_contact_author_name 'Dr Sundargopal Ghosh' _publ_contact_author_address ; Chemistry and Biochemistry University of Notre Dame South Bend IN, USA Indiana 46556 UNITED STATES OF AMERICA ; _publ_contact_author_email SGHOSH@ND.EDU loop_ _publ_author_name _publ_author_footnote _publ_author_address S.Ghosh ; ? ; ; Department of Chemistry and Biochemistry University of Notre Dame Notre Dame, IN 46556-5670 ; B.C.Noll ; ? ; ; Department of Chemistry and Biochemistry University of Notre Dame Notre Dame, IN 46556-5670 ; T.P.Fehlner ; ? ; ; Department of Chemistry and Biochemistry University of Notre Dame Notre Dame, IN 46556-5670 ; _publ_section_title ; Condensed metallaborane clusters: Synthesis and structure of Fe2(CO)6(h5-C5Me5RuCO)(h5-C5Me5Ru)B6H10 ; data_bcn03 _database_code_depnum_ccdc_archive 'CCDC 234013' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H40 B6 Fe2 O7 Ru2' _chemical_formula_sum 'C27 H40 B6 Fe2 O7 Ru2' _chemical_formula_weight 855.29 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' Ru Ru -1.2594 0.8363 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6024(10) _cell_length_b 22.536(2) _cell_length_c 16.0264(16) _cell_angle_alpha 90.00 _cell_angle_beta 99.642(2) _cell_angle_gamma 90.00 _cell_volume 3419.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6594 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 31.489 _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 1.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5430 _exptl_absorpt_correction_T_max 0.7224 _exptl_absorpt_process_details 'Blessing, R. H. Acta Cryst. (1995) A51. 33-8.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37171 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 31.52 _reflns_number_total 11326 _reflns_number_gt 9279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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. Methyl hydrogen atoms were placed at calculated geometries and allowed to ride on the position of the parent atom. Isotropic thermal parameters for these hydrogens were calculated at1.2 times the equivalent isotropic thermal parameterof the parent atom. All hydrogens bound to the boron framework were located by difference electron density map and were freely refined. ; _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^)+(0.0343P)^2^+8.4631P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11326 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1134 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.168 _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 Ru1 Ru 0.10751(3) 0.109730(13) 0.817937(18) 0.01197(7) Uani 1 1 d . . . Ru2 Ru 0.27007(3) 0.124234(12) 0.603130(18) 0.01034(6) Uani 1 1 d . . . Fe2 Fe 0.16241(6) 0.27530(2) 0.71625(3) 0.01389(11) Uani 1 1 d . . . Fe1 Fe 0.40631(7) 0.25334(2) 0.80392(3) 0.01541(12) Uani 1 1 d . . . B1 B 0.2153(5) 0.19321(19) 0.7868(3) 0.0140(8) Uani 1 1 d . . . H11 H 0.303(5) 0.208(2) 0.850(3) 0.023(13) Uiso 1 1 d . . . H12 H 0.115(7) 0.236(3) 0.784(4) 0.06(2) Uiso 1 1 d . . . B2 B 0.2895(5) 0.20003(18) 0.6974(3) 0.0126(8) Uani 1 1 d . . . H21 H 0.418(5) 0.219(2) 0.716(3) 0.024(13) Uiso 1 1 d . . . H22 H 0.249(6) 0.193(2) 0.609(3) 0.034(15) Uiso 1 1 d . . . B3 B 0.2819(5) 0.12831(18) 0.7432(3) 0.0135(8) Uani 1 1 d . . . H3 H 0.387(5) 0.112(2) 0.785(3) 0.016(12) Uiso 1 1 d . . . B4 B 0.1695(5) 0.07000(19) 0.6961(3) 0.0136(8) Uani 1 1 d . . . H4 H 0.212(6) 0.028(2) 0.709(3) 0.027(14) Uiso 1 1 d . . . B5 B -0.0084(5) 0.0785(2) 0.6962(3) 0.0166(8) Uani 1 1 d . . . H5 H -0.095(6) 0.047(2) 0.701(3) 0.027(14) Uiso 1 1 d . . . H56 H -0.047(5) 0.113(2) 0.636(3) 0.014(12) Uiso 1 1 d . . . B6 B 0.0552(5) 0.0892(2) 0.6024(3) 0.0169(8) Uani 1 1 d . . . H6 H 0.005(6) 0.062(2) 0.552(3) 0.025(13) Uiso 1 1 d . . . H62 H 0.104(5) 0.146(2) 0.568(3) 0.017(12) Uiso 1 1 d . . . O1 O -0.1492(4) 0.18760(15) 0.7752(2) 0.0270(7) Uani 1 1 d . . . O2 O 0.6486(4) 0.19448(17) 0.9080(2) 0.0350(8) Uani 1 1 d . . . O3 O 0.5783(4) 0.33781(14) 0.7274(2) 0.0275(7) Uani 1 1 d . . . O4 O 0.3279(4) 0.34027(16) 0.9241(2) 0.0366(9) Uani 1 1 d . . . O5 O 0.2847(4) 0.33845(16) 0.5871(2) 0.0334(8) Uani 1 1 d . . . O6 O 0.0404(5) 0.38111(15) 0.7857(2) 0.0403(10) Uani 1 1 d . . . O7 O -0.0876(4) 0.24300(15) 0.5928(2) 0.0334(8) Uani 1 1 d . . . C1 C 0.2454(5) 0.08966(18) 0.9458(2) 0.0189(8) Uani 1 1 d . . . C2 C 0.2294(5) 0.03594(17) 0.8983(2) 0.0186(8) Uani 1 1 d . . . C3 C 0.0829(5) 0.02118(17) 0.8806(2) 0.0176(8) Uani 1 1 d . . . C4 C 0.0070(5) 0.06597(17) 0.9174(2) 0.0174(8) Uani 1 1 d . . . C5 C 0.1086(5) 0.10879(17) 0.9566(2) 0.0170(8) Uani 1 1 d . . . C6 C 0.3835(5) 0.1179(2) 0.9838(3) 0.0270(10) Uani 1 1 d . . . H6A H 0.4234 0.0969 1.0359 0.032 Uiso 1 1 calc R . . H6B H 0.3674 0.1596 0.9970 0.032 Uiso 1 1 calc R . . H6C H 0.4494 0.1157 0.9434 0.032 Uiso 1 1 calc R . . C7 C 0.3477(6) -0.0020(2) 0.8787(3) 0.0286(10) Uani 1 1 d . . . H7A H 0.4357 0.0209 0.8878 0.034 Uiso 1 1 calc R . . H7B H 0.3268 -0.0150 0.8196 0.034 Uiso 1 1 calc R . . H7C H 0.3582 -0.0368 0.9159 0.034 Uiso 1 1 calc R . . C8 C 0.0224(6) -0.03396(18) 0.8384(3) 0.0264(10) Uani 1 1 d . . . H8A H 0.0254 -0.0657 0.8804 0.032 Uiso 1 1 calc R . . H8B H 0.0776 -0.0458 0.7949 0.032 Uiso 1 1 calc R . . H8C H -0.0758 -0.0268 0.8119 0.032 Uiso 1 1 calc R . . C9 C -0.1486(5) 0.0646(2) 0.9196(3) 0.0246(9) Uani 1 1 d . . . H9A H -0.1668 0.0384 0.9655 0.030 Uiso 1 1 calc R . . H9B H -0.1990 0.0496 0.8655 0.030 Uiso 1 1 calc R . . H9C H -0.1815 0.1047 0.9293 0.030 Uiso 1 1 calc R . . C10 C 0.0791(6) 0.16185(19) 1.0082(3) 0.0254(9) Uani 1 1 d . . . H10A H 0.0816 0.1498 1.0672 0.030 Uiso 1 1 calc R . . H10B H -0.0144 0.1779 0.9855 0.030 Uiso 1 1 calc R . . H10C H 0.1510 0.1923 1.0055 0.030 Uiso 1 1 calc R . . C11 C 0.3499(4) 0.04332(17) 0.5458(2) 0.0149(7) Uani 1 1 d . . . C12 C 0.4642(4) 0.07061(17) 0.6022(2) 0.0159(7) Uani 1 1 d . . . C13 C 0.4852(4) 0.12862(18) 0.5709(3) 0.0186(8) Uani 1 1 d . . . C14 C 0.3853(5) 0.13773(17) 0.4953(3) 0.0181(8) Uani 1 1 d . . . C15 C 0.3017(5) 0.08507(17) 0.4797(2) 0.0168(8) Uani 1 1 d . . . C16 C 0.3024(5) -0.01989(18) 0.5500(3) 0.0218(8) Uani 1 1 d . . . H16A H 0.2032 -0.0232 0.5232 0.026 Uiso 1 1 calc R . . H16B H 0.3123 -0.0323 0.6094 0.026 Uiso 1 1 calc R . . H16C H 0.3606 -0.0454 0.5203 0.026 Uiso 1 1 calc R . . C17 C 0.5529(5) 0.0413(2) 0.6772(3) 0.0259(9) Uani 1 1 d . . . H17A H 0.6264 0.0172 0.6580 0.031 Uiso 1 1 calc R . . H17B H 0.4930 0.0158 0.7059 0.031 Uiso 1 1 calc R . . H17C H 0.5971 0.0717 0.7167 0.031 Uiso 1 1 calc R . . C18 C 0.6021(5) 0.1705(2) 0.6057(3) 0.0302(11) Uani 1 1 d . . . H18A H 0.6826 0.1643 0.5764 0.036 Uiso 1 1 calc R . . H18B H 0.6314 0.1630 0.6664 0.036 Uiso 1 1 calc R . . H18C H 0.5687 0.2114 0.5972 0.036 Uiso 1 1 calc R . . C19 C 0.3798(6) 0.1909(2) 0.4379(3) 0.0303(11) Uani 1 1 d . . . H19A H 0.3683 0.2270 0.4701 0.036 Uiso 1 1 calc R . . H19B H 0.2998 0.1869 0.3914 0.036 Uiso 1 1 calc R . . H19C H 0.4678 0.1934 0.4147 0.036 Uiso 1 1 calc R . . C20 C 0.1864(5) 0.0749(2) 0.4055(3) 0.0258(10) Uani 1 1 d . . . H20A H 0.1265 0.1102 0.3961 0.031 Uiso 1 1 calc R . . H20B H 0.1291 0.0408 0.4171 0.031 Uiso 1 1 calc R . . H20C H 0.2282 0.0669 0.3549 0.031 Uiso 1 1 calc R . . C21 C -0.0491(5) 0.15806(18) 0.7867(3) 0.0185(8) Uani 1 1 d . . . C22 C 0.5544(5) 0.21659(19) 0.8668(3) 0.0229(9) Uani 1 1 d . . . C23 C 0.5085(5) 0.30564(17) 0.7568(2) 0.0187(8) Uani 1 1 d . . . C24 C 0.3564(5) 0.3067(2) 0.8771(3) 0.0257(10) Uani 1 1 d . . . C25 C 0.2366(5) 0.31414(18) 0.6389(3) 0.0194(8) Uani 1 1 d . . . C26 C 0.0899(5) 0.33942(18) 0.7614(3) 0.0225(9) Uani 1 1 d . . . C27 C 0.0082(5) 0.25545(18) 0.6431(3) 0.0212(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01502(15) 0.01083(12) 0.01021(13) 0.00086(10) 0.00252(10) -0.00030(10) Ru2 0.00997(14) 0.01168(12) 0.00909(12) -0.00069(9) 0.00077(10) -0.00053(10) Fe2 0.0185(3) 0.0112(2) 0.0122(2) -0.00002(18) 0.0033(2) -0.0002(2) Fe1 0.0187(3) 0.0142(2) 0.0122(2) -0.00139(19) -0.0006(2) -0.0042(2) B1 0.017(2) 0.0136(18) 0.0113(17) -0.0002(14) 0.0005(16) -0.0013(15) B2 0.012(2) 0.0142(18) 0.0113(17) -0.0009(14) 0.0005(15) -0.0051(14) B3 0.015(2) 0.0119(17) 0.0129(17) -0.0012(14) 0.0014(15) -0.0038(15) B4 0.013(2) 0.0136(18) 0.0142(19) -0.0020(14) 0.0024(15) -0.0012(15) B5 0.016(2) 0.019(2) 0.0149(19) -0.0029(15) 0.0007(16) -0.0027(16) B6 0.013(2) 0.022(2) 0.0152(19) -0.0004(16) 0.0011(16) -0.0017(16) O1 0.0227(17) 0.0293(17) 0.0291(17) 0.0050(13) 0.0048(14) 0.0071(13) O2 0.0249(19) 0.040(2) 0.036(2) 0.0101(16) -0.0053(16) -0.0029(15) O3 0.036(2) 0.0247(16) 0.0217(15) 0.0016(12) 0.0031(14) -0.0122(14) O4 0.048(2) 0.0306(18) 0.0320(19) -0.0147(15) 0.0083(17) -0.0010(16) O5 0.038(2) 0.042(2) 0.0218(16) 0.0092(14) 0.0070(15) -0.0082(16) O6 0.058(3) 0.0242(17) 0.042(2) -0.0042(15) 0.017(2) 0.0119(17) O7 0.0277(19) 0.0306(18) 0.037(2) 0.0049(14) -0.0079(16) -0.0035(14) C1 0.026(2) 0.0193(18) 0.0117(17) 0.0067(14) 0.0035(16) 0.0023(16) C2 0.026(2) 0.0181(17) 0.0126(16) 0.0065(14) 0.0045(15) 0.0051(16) C3 0.024(2) 0.0124(16) 0.0161(17) 0.0039(13) 0.0038(16) -0.0005(14) C4 0.023(2) 0.0172(17) 0.0130(17) 0.0060(13) 0.0061(15) -0.0010(15) C5 0.025(2) 0.0157(17) 0.0105(16) 0.0040(13) 0.0044(15) 0.0011(15) C6 0.021(2) 0.031(2) 0.026(2) 0.0064(18) -0.0061(18) -0.0047(18) C7 0.034(3) 0.026(2) 0.027(2) 0.0085(17) 0.008(2) 0.0120(19) C8 0.036(3) 0.0152(18) 0.028(2) 0.0036(16) 0.004(2) -0.0029(17) C9 0.022(2) 0.029(2) 0.024(2) 0.0094(17) 0.0089(18) -0.0007(17) C10 0.037(3) 0.0204(19) 0.021(2) -0.0034(16) 0.0103(19) 0.0012(18) C11 0.0138(19) 0.0167(17) 0.0151(17) -0.0036(13) 0.0053(14) 0.0002(14) C12 0.0137(19) 0.0188(18) 0.0158(17) -0.0019(14) 0.0044(14) 0.0028(14) C13 0.016(2) 0.0179(17) 0.025(2) -0.0053(15) 0.0122(16) -0.0048(15) C14 0.025(2) 0.0164(17) 0.0164(17) 0.0000(14) 0.0119(16) 0.0036(15) C15 0.021(2) 0.0191(18) 0.0116(16) -0.0021(13) 0.0064(15) 0.0049(15) C16 0.022(2) 0.0172(18) 0.027(2) -0.0021(15) 0.0063(18) 0.0020(15) C17 0.015(2) 0.038(3) 0.024(2) 0.0006(18) -0.0003(17) 0.0063(18) C18 0.016(2) 0.034(2) 0.043(3) -0.012(2) 0.012(2) -0.0142(18) C19 0.048(3) 0.020(2) 0.027(2) 0.0037(17) 0.020(2) 0.002(2) C20 0.031(3) 0.030(2) 0.0145(18) -0.0074(16) -0.0030(17) 0.0084(19) C21 0.018(2) 0.0196(18) 0.0187(18) 0.0003(14) 0.0062(16) -0.0016(15) C22 0.021(2) 0.023(2) 0.023(2) 0.0013(16) 0.0005(17) -0.0063(16) C23 0.024(2) 0.0170(17) 0.0132(17) -0.0021(13) -0.0034(15) -0.0029(15) C24 0.034(3) 0.021(2) 0.022(2) -0.0042(16) 0.0062(19) -0.0072(18) C25 0.018(2) 0.0216(19) 0.0170(18) 0.0006(14) -0.0004(16) -0.0010(15) C26 0.026(2) 0.0177(18) 0.025(2) -0.0003(15) 0.0072(18) 0.0011(16) C27 0.017(2) 0.0179(18) 0.027(2) 0.0034(15) 0.0011(17) -0.0010(15) _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 Ru1 C21 1.856(4) . ? Ru1 B5 2.194(4) . ? Ru1 C5 2.221(4) . ? Ru1 C4 2.228(4) . ? Ru1 B1 2.243(4) . ? Ru1 B3 2.255(4) . ? Ru1 C3 2.264(4) . ? Ru1 C1 2.291(4) . ? Ru1 C2 2.300(4) . ? Ru1 B4 2.315(4) . ? Ru2 B6 2.207(5) . ? Ru2 C13 2.214(4) . ? Ru2 C14 2.223(4) . ? Ru2 C12 2.224(4) . ? Ru2 B3 2.231(4) . ? Ru2 C15 2.233(4) . ? Ru2 C11 2.234(4) . ? Ru2 B4 2.264(4) . ? Ru2 B2 2.267(4) . ? Ru2 H22 1.56(5) . ? Ru2 H62 1.68(5) . ? Fe2 C25 1.763(4) . ? Fe2 C27 1.784(4) . ? Fe2 C26 1.807(4) . ? Fe2 B2 2.141(4) . ? Fe2 B1 2.183(4) . ? Fe2 Fe1 2.5694(9) . ? Fe2 H12 1.53(6) . ? Fe1 C23 1.781(4) . ? Fe1 C24 1.800(5) . ? Fe1 C22 1.801(5) . ? Fe1 B2 2.231(4) . ? Fe1 B1 2.260(5) . ? Fe1 H11 1.67(5) . ? Fe1 H21 1.63(5) . ? B1 B2 1.711(6) . ? B1 B3 1.785(6) . ? B1 H11 1.24(5) . ? B1 H12 1.36(7) . ? B2 B3 1.782(6) . ? B2 H21 1.29(5) . ? B2 H22 1.42(5) . ? B3 B4 1.786(6) . ? B3 H3 1.18(5) . ? B4 B5 1.719(7) . ? B4 B6 1.759(6) . ? B4 H4 1.03(5) . ? B5 B6 1.732(7) . ? B5 H5 1.11(5) . ? B5 H56 1.25(4) . ? B6 H56 1.31(5) . ? B6 H6 1.06(5) . ? B6 H62 1.50(5) . ? O1 C21 1.158(5) . ? O2 C22 1.141(5) . ? O3 C23 1.141(5) . ? O4 C24 1.133(5) . ? O5 C25 1.154(5) . ? O6 C26 1.151(5) . ? O7 C27 1.152(5) . ? C1 C5 1.421(6) . ? C1 C2 1.424(6) . ? C1 C6 1.505(6) . ? C2 C3 1.427(6) . ? C2 C7 1.497(6) . ? C3 C4 1.430(6) . ? C3 C8 1.486(6) . ? C4 C5 1.440(6) . ? C4 C9 1.500(6) . ? C5 C10 1.507(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C15 1.435(5) . ? C11 C12 1.438(5) . ? C11 C16 1.501(6) . ? C12 C13 1.427(6) . ? C12 C17 1.505(6) . ? C13 C14 1.429(6) . ? C13 C18 1.500(6) . ? C14 C15 1.431(6) . ? C14 C19 1.506(6) . ? C15 C20 1.500(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Ru1 B5 71.39(18) . . ? C21 Ru1 C5 98.25(17) . . ? B5 Ru1 C5 143.47(17) . . ? C21 Ru1 C4 91.39(17) . . ? B5 Ru1 C4 106.16(17) . . ? C5 Ru1 C4 37.76(15) . . ? C21 Ru1 B1 80.26(17) . . ? B5 Ru1 B1 104.80(16) . . ? C5 Ru1 B1 107.79(15) . . ? C4 Ru1 B1 143.30(15) . . ? C21 Ru1 B3 112.81(17) . . ? B5 Ru1 B3 84.18(17) . . ? C5 Ru1 B3 130.82(16) . . ? C4 Ru1 B3 155.74(16) . . ? B1 Ru1 B3 46.75(16) . . ? C21 Ru1 C3 119.79(17) . . ? B5 Ru1 C3 92.09(16) . . ? C5 Ru1 C3 62.04(14) . . ? C4 Ru1 C3 37.11(15) . . ? B1 Ru1 C3 157.54(16) . . ? B3 Ru1 C3 122.76(16) . . ? C21 Ru1 C1 132.70(17) . . ? B5 Ru1 C1 149.68(16) . . ? C5 Ru1 C1 36.68(15) . . ? C4 Ru1 C1 61.80(16) . . ? B1 Ru1 C1 98.36(15) . . ? B3 Ru1 C1 98.17(16) . . ? C3 Ru1 C1 61.12(15) . . ? C21 Ru1 C2 152.70(17) . . ? B5 Ru1 C2 113.62(16) . . ? C5 Ru1 C2 61.06(15) . . ? C4 Ru1 C2 61.32(16) . . ? B1 Ru1 C2 121.37(16) . . ? B3 Ru1 C2 94.48(16) . . ? C3 Ru1 C2 36.43(15) . . ? C1 Ru1 C2 36.15(14) . . ? C21 Ru1 B4 108.07(17) . . ? B5 Ru1 B4 44.72(17) . . ? C5 Ru1 B4 151.86(15) . . ? C4 Ru1 B4 129.50(15) . . ? B1 Ru1 B4 86.75(15) . . ? B3 Ru1 B4 45.99(15) . . ? C3 Ru1 B4 95.39(15) . . ? C1 Ru1 B4 119.10(15) . . ? C2 Ru1 B4 90.81(15) . . ? B6 Ru2 C13 157.31(16) . . ? B6 Ru2 C14 129.14(17) . . ? C13 Ru2 C14 37.57(16) . . ? B6 Ru2 C12 126.12(16) . . ? C13 Ru2 C12 37.51(15) . . ? C14 Ru2 C12 62.78(15) . . ? B6 Ru2 B3 84.85(16) . . ? C13 Ru2 B3 109.91(16) . . ? C14 Ru2 B3 145.94(16) . . ? C12 Ru2 B3 97.31(15) . . ? B6 Ru2 C15 96.87(17) . . ? C13 Ru2 C15 62.63(16) . . ? C14 Ru2 C15 37.47(15) . . ? C12 Ru2 C15 62.67(15) . . ? B3 Ru2 C15 156.40(15) . . ? B6 Ru2 C11 95.20(16) . . ? C13 Ru2 C11 62.79(14) . . ? C14 Ru2 C11 62.78(14) . . ? C12 Ru2 C11 37.64(14) . . ? B3 Ru2 C11 118.96(15) . . ? C15 Ru2 C11 37.47(14) . . ? B6 Ru2 B4 46.30(16) . . ? C13 Ru2 B4 134.03(16) . . ? C14 Ru2 B4 155.19(15) . . ? C12 Ru2 B4 99.28(15) . . ? B3 Ru2 B4 46.82(15) . . ? C15 Ru2 B4 120.37(15) . . ? C11 Ru2 B4 92.48(15) . . ? B6 Ru2 B2 104.22(17) . . ? C13 Ru2 B2 98.39(15) . . ? C14 Ru2 B2 114.74(15) . . ? C12 Ru2 B2 115.99(15) . . ? B3 Ru2 B2 46.67(15) . . ? C15 Ru2 B2 151.63(15) . . ? C11 Ru2 B2 153.28(15) . . ? B4 Ru2 B2 88.00(15) . . ? B6 Ru2 H22 103(2) . . ? C13 Ru2 H22 96(2) . . ? C14 Ru2 H22 90(2) . . ? C12 Ru2 H22 131(2) . . ? B3 Ru2 H22 83.6(19) . . ? C15 Ru2 H22 118.6(19) . . ? C11 Ru2 H22 152(2) . . ? B4 Ru2 H22 115(2) . . ? B2 Ru2 H22 38.3(19) . . ? B6 Ru2 H62 42.7(16) . . ? C13 Ru2 H62 141.6(16) . . ? C14 Ru2 H62 105.7(16) . . ? C12 Ru2 H62 155.5(16) . . ? B3 Ru2 H62 102.1(16) . . ? C15 Ru2 H62 94.7(16) . . ? C11 Ru2 H62 118.3(16) . . ? B4 Ru2 H62 83.7(16) . . ? B2 Ru2 H62 88.3(16) . . ? H22 Ru2 H62 67(3) . . ? C25 Fe2 C27 92.9(2) . . ? C25 Fe2 C26 96.5(2) . . ? C27 Fe2 C26 97.5(2) . . ? C25 Fe2 B2 89.25(18) . . ? C27 Fe2 B2 97.95(18) . . ? C26 Fe2 B2 163.23(19) . . ? C25 Fe2 B1 134.32(19) . . ? C27 Fe2 B1 102.89(18) . . ? C26 Fe2 B1 122.84(18) . . ? B2 Fe2 B1 46.61(16) . . ? C25 Fe2 Fe1 92.36(14) . . ? C27 Fe2 Fe1 152.98(14) . . ? C26 Fe2 Fe1 108.21(15) . . ? B2 Fe2 Fe1 55.64(11) . . ? B1 Fe2 Fe1 56.08(12) . . ? C25 Fe2 H12 172(2) . . ? C27 Fe2 H12 90(2) . . ? C26 Fe2 H12 90(2) . . ? B2 Fe2 H12 83(2) . . ? B1 Fe2 H12 38(2) . . ? Fe1 Fe2 H12 82(3) . . ? C23 Fe1 C24 93.4(2) . . ? C23 Fe1 C22 95.9(2) . . ? C24 Fe1 C22 102.4(2) . . ? C23 Fe1 B2 105.89(16) . . ? C24 Fe1 B2 134.8(2) . . ? C22 Fe1 B2 115.42(18) . . ? C23 Fe1 B1 147.04(17) . . ? C24 Fe1 B1 100.42(19) . . ? C22 Fe1 B1 109.92(18) . . ? B2 Fe1 B1 44.79(16) . . ? C23 Fe1 Fe2 99.05(14) . . ? C24 Fe1 Fe2 84.82(16) . . ? C22 Fe1 Fe2 163.03(14) . . ? B2 Fe1 Fe2 52.39(12) . . ? B1 Fe1 Fe2 53.28(11) . . ? C23 Fe1 H11 176.0(17) . . ? C24 Fe1 H11 83.1(17) . . ? C22 Fe1 H11 86.9(17) . . ? B2 Fe1 H11 75.4(17) . . ? B1 Fe1 H11 32.8(17) . . ? Fe2 Fe1 H11 78.6(17) . . ? C23 Fe1 H21 80.1(18) . . ? C24 Fe1 H21 161.2(18) . . ? C22 Fe1 H21 95.8(18) . . ? B2 Fe1 H21 34.8(18) . . ? B1 Fe1 H21 77.2(18) . . ? Fe2 Fe1 H21 78.9(18) . . ? H11 Fe1 H21 103(2) . . ? B2 B1 B3 61.2(2) . . ? B2 B1 Fe2 65.4(2) . . ? B3 B1 Fe2 124.0(3) . . ? B2 B1 Ru1 122.3(3) . . ? B3 B1 Ru1 66.98(19) . . ? Fe2 B1 Ru1 138.6(2) . . ? B2 B1 Fe1 66.7(2) . . ? B3 B1 Fe1 101.6(3) . . ? Fe2 B1 Fe1 70.63(13) . . ? Ru1 B1 Fe1 150.6(2) . . ? B2 B1 H11 109(2) . . ? B3 B1 H11 107(2) . . ? Fe2 B1 H11 105(2) . . ? Ru1 B1 H11 109(2) . . ? Fe1 B1 H11 47(2) . . ? B2 B1 H12 108(3) . . ? B3 B1 H12 150(3) . . ? Fe2 B1 H12 44(3) . . ? Ru1 B1 H12 104(3) . . ? Fe1 B1 H12 98(3) . . ? H11 B1 H12 103(4) . . ? B1 B2 B3 61.4(2) . . ? B1 B2 Fe2 68.0(2) . . ? B3 B2 Fe2 126.6(3) . . ? B1 B2 Fe1 68.5(2) . . ? B3 B2 Fe1 102.9(2) . . ? Fe2 B2 Fe1 71.97(13) . . ? B1 B2 Ru2 119.4(3) . . ? B3 B2 Ru2 65.60(19) . . ? Fe2 B2 Ru2 134.9(2) . . ? Fe1 B2 Ru2 152.9(2) . . ? B1 B2 H21 111(2) . . ? B3 B2 H21 108(2) . . ? Fe2 B2 H21 105(2) . . ? Fe1 B2 H21 46(2) . . ? Ru2 B2 H21 112(2) . . ? B1 B2 H22 138(2) . . ? B3 B2 H22 106(2) . . ? Fe2 B2 H22 100(2) . . ? Fe1 B2 H22 148(2) . . ? Ru2 B2 H22 43(2) . . ? H21 B2 H22 111(3) . . ? B2 B3 B1 57.3(2) . . ? B2 B3 B4 123.8(3) . . ? B1 B3 B4 122.5(3) . . ? B2 B3 Ru2 67.74(19) . . ? B1 B3 Ru2 117.8(2) . . ? B4 B3 Ru2 67.57(19) . . ? B2 B3 Ru1 118.2(3) . . ? B1 B3 Ru1 66.3(2) . . ? B4 B3 Ru1 68.8(2) . . ? Ru2 B3 Ru1 127.6(2) . . ? B2 B3 H3 115(2) . . ? B1 B3 H3 111(2) . . ? B4 B3 H3 114(2) . . ? Ru2 B3 H3 117(2) . . ? Ru1 B3 H3 106(2) . . ? B5 B4 B6 59.7(3) . . ? B5 B4 B3 116.6(3) . . ? B6 B4 B3 115.3(3) . . ? B5 B4 Ru2 118.3(3) . . ? B6 B4 Ru2 65.1(2) . . ? B3 B4 Ru2 65.60(19) . . ? B5 B4 Ru1 63.9(2) . . ? B6 B4 Ru1 114.4(3) . . ? B3 B4 Ru1 65.23(19) . . ? Ru2 B4 Ru1 122.98(18) . . ? B5 B4 H4 118(3) . . ? B6 B4 H4 124(3) . . ? B3 B4 H4 113(3) . . ? Ru2 B4 H4 115(3) . . ? Ru1 B4 H4 110(3) . . ? B4 B5 B6 61.3(3) . . ? B4 B5 Ru1 71.4(2) . . ? B6 B5 Ru1 121.8(3) . . ? B4 B5 H5 133(3) . . ? B6 B5 H5 122(3) . . ? Ru1 B5 H5 115(3) . . ? B4 B5 H56 103(2) . . ? B6 B5 H56 49(2) . . ? Ru1 B5 H56 122(2) . . ? H5 B5 H56 109(3) . . ? B5 B6 B4 59.0(3) . . ? B5 B6 Ru2 120.7(3) . . ? B4 B6 Ru2 68.6(2) . . ? B5 B6 H56 46(2) . . ? B4 B6 H56 99(2) . . ? Ru2 B6 H56 128(2) . . ? B5 B6 H6 114(3) . . ? B4 B6 H6 130(3) . . ? Ru2 B6 H6 121(3) . . ? H56 B6 H6 106(4) . . ? B5 B6 H62 127.9(18) . . ? B4 B6 H62 109.6(18) . . ? Ru2 B6 H62 49.4(18) . . ? H56 B6 H62 96(3) . . ? H6 B6 H62 110(3) . . ? C5 C1 C2 107.7(4) . . ? C5 C1 C6 126.3(4) . . ? C2 C1 C6 125.8(4) . . ? C5 C1 Ru1 69.0(2) . . ? C2 C1 Ru1 72.3(2) . . ? C6 C1 Ru1 128.1(3) . . ? C1 C2 C3 108.6(4) . . ? C1 C2 C7 125.4(4) . . ? C3 C2 C7 125.6(4) . . ? C1 C2 Ru1 71.6(2) . . ? C3 C2 Ru1 70.4(2) . . ? C7 C2 Ru1 129.0(3) . . ? C2 C3 C4 107.9(4) . . ? C2 C3 C8 125.7(4) . . ? C4 C3 C8 126.2(4) . . ? C2 C3 Ru1 73.1(2) . . ? C4 C3 Ru1 70.1(2) . . ? C8 C3 Ru1 126.7(3) . . ? C3 C4 C5 107.3(4) . . ? C3 C4 C9 125.0(4) . . ? C5 C4 C9 127.5(4) . . ? C3 C4 Ru1 72.8(2) . . ? C5 C4 Ru1 70.8(2) . . ? C9 C4 Ru1 125.4(3) . . ? C1 C5 C4 108.5(4) . . ? C1 C5 C10 124.8(4) . . ? C4 C5 C10 126.5(4) . . ? C1 C5 Ru1 74.3(2) . . ? C4 C5 Ru1 71.4(2) . . ? C10 C5 Ru1 124.9(3) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C15 C11 C12 107.6(3) . . ? C15 C11 C16 126.4(4) . . ? C12 C11 C16 125.7(4) . . ? C15 C11 Ru2 71.2(2) . . ? C12 C11 Ru2 70.8(2) . . ? C16 C11 Ru2 128.9(3) . . ? C13 C12 C11 108.0(3) . . ? C13 C12 C17 126.1(4) . . ? C11 C12 C17 125.8(4) . . ? C13 C12 Ru2 70.9(2) . . ? C11 C12 Ru2 71.6(2) . . ? C17 C12 Ru2 126.6(3) . . ? C12 C13 C14 108.4(3) . . ? C12 C13 C18 125.9(4) . . ? C14 C13 C18 125.4(4) . . ? C12 C13 Ru2 71.6(2) . . ? C14 C13 Ru2 71.6(2) . . ? C18 C13 Ru2 127.6(3) . . ? C13 C14 C15 107.8(3) . . ? C13 C14 C19 125.6(4) . . ? C15 C14 C19 126.2(4) . . ? C13 C14 Ru2 70.9(2) . . ? C15 C14 Ru2 71.6(2) . . ? C19 C14 Ru2 127.8(3) . . ? C14 C15 C11 108.2(4) . . ? C14 C15 C20 125.7(4) . . ? C11 C15 C20 126.1(4) . . ? C14 C15 Ru2 70.9(2) . . ? C11 C15 Ru2 71.3(2) . . ? C20 C15 Ru2 124.8(3) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O1 C21 Ru1 173.3(4) . . ? O2 C22 Fe1 178.3(4) . . ? O3 C23 Fe1 177.5(4) . . ? O4 C24 Fe1 178.5(5) . . ? O5 C25 Fe2 178.4(4) . . ? O6 C26 Fe2 176.3(4) . . ? O7 C27 Fe2 176.7(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 31.52 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.646 _refine_diff_density_min -1.224 _refine_diff_density_rms 0.164 #============================================================================== # Additional structures (last six sections and associated data_? identifiers) # may be added at this point. #==============================================================================