# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1619 data_global _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_section_title ; Ferratricarbollide Design for Molecular Assamblies: Complexes [closo-9,9'-(Bu^t^HN)~2~-commo-2,2'-M-1,7,9-(C~3~B~8~H~10~)-1',7',9'- (C~3~B~8~H~10~)] (where M = Fe and Ru), the First Examples of Double-Cluster Metallatricarbollides. ; _publ_contact_letter ; Please consider this CIF submission as crystallographic information file for paper ref. 9/05606H. Crystallographic data for the structures reported in this paper have been deposited at the Cambridge Crystallographic Data Centre with reference numbers CCDC-112859 and CCDC-112860. ; _publ_contact_author ; Dr Bohumil Stibr, DSc Institute of Inorganic Chemistry Academy of Sciences of the Czech Republic 25056 Rez Czech Republic ; _publ_contact_author_phone '+4202-66173109' _publ_contact_author_fax '+4202-20941502' _publ_contact_author_email 'stibr@iic.cas.cz' loop_ _publ_author_name _publ_author_address 'Bohumir Gr\~uner' ; Institute of Material Sciences Campus UAB 08193 Bellaterra Spain ; 'Francesc Teixidor' ; Institute of Material Sciences Campus UAB 08193 Bellaterra Spain ; 'Clara Vi\~nas' ; Institute of Material Sciences Campus UAB 08193 Bellaterra Spain ; 'Sillanp\"a\"a, R.' ; Department of Chemistry University of Turku FIN-20014 Turku Finland ; 'Raikko Kivek\"as' ; Department of Chemistry P.O.Box 55 FIN-00014 University of Helsinki Finland ; 'Bohumil \2sigma(I) _computing_data_collection ; MSC/AFC5S Control Program (Molecular Structure Corporation, 1995) ; _computing_cell_refinement ; MSC/AFC5S Control Program (Molecular Structure Corporation, 1995) ; _computing_data_reduction ; TEXSAN (Molecular Structure Corporation, 1989) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Carbon and boron atoms at the coordinated C~2~B~3~ faces could not very reliable distinguished. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+0.3069P] 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 0.04(3) _refine_ls_number_reflns 2339 _refine_ls_number_parameters 309 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.1013 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.039 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N N 0.1476(3) 0.8561(3) 0.2174(2) 0.0421(9) Uani 1 d D . . H0 H 0.0695(4) 0.858(3) 0.2080(7) 0.051 Uiso 1 d D . . C1 C 0.0971(4) 0.8450(4) 0.4325(3) 0.0434(11) Uani 1 d . . . H1 H 0.0218 0.8154 0.4657 0.052 Uiso 1 calc R . . Fe2 Fe 0.23181(4) 0.90168(4) 0.5000 0.03199(17) Uani 1 d . . . B3 B 0.1227(5) 0.9760(4) 0.4255(3) 0.0395(13) Uani 1 d . . . H3 H 0.0684 1.0354 0.4542 0.047 Uiso 1 calc R . . B4 B 0.0633(5) 0.9058(4) 0.3499(3) 0.0444(13) Uani 1 d . . . H4 H -0.0281 0.9194 0.3297 0.053 Uiso 1 calc R . . B5 B 0.1287(4) 0.7785(4) 0.3517(3) 0.0421(12) Uani 1 d . . . H5 H 0.0804 0.7080 0.3329 0.051 Uiso 1 calc R . . B6 B 0.2289(5) 0.7756(4) 0.4289(3) 0.0388(12) Uani 1 d . . . H6 H 0.2458 0.7023 0.4595 0.047 Uiso 1 calc R . . C7 C 0.2731(4) 0.9905(4) 0.4084(3) 0.0450(12) Uani 1 d . . . H7 H 0.3218 1.0619 0.4249 0.054 Uiso 1 calc R . . B8 B 0.1741(6) 0.9984(5) 0.3334(3) 0.0423(15) Uani 1 d . . . H8 H 0.1565 1.0716 0.3028 0.051 Uiso 1 calc R . . C9 C 0.1791(4) 0.8733(4) 0.2930(3) 0.0357(10) Uani 1 d D . . B10 B 0.2822(6) 0.7931(5) 0.3363(3) 0.0384(14) Uani 1 d . . . H10 H 0.3348 0.7327 0.3074 0.046 Uiso 1 calc R . . B11 B 0.3373(5) 0.8675(4) 0.4094(3) 0.0342(12) Uani 1 d . . . H11 H 0.4306 0.8551 0.4265 0.041 Uiso 1 calc R . . B12 B 0.3114(5) 0.9278(5) 0.3239(3) 0.0401(13) Uani 1 d . . . H12 H 0.3831 0.9552 0.2869 0.048 Uiso 1 calc R . . C13 C 0.2149(4) 0.8847(4) 0.1498(3) 0.0429(11) Uani 1 d D . . C14 C 0.1373(5) 0.8463(4) 0.0858(3) 0.0539(13) Uani 1 d . . . H14A H 0.1324 0.7710 0.0871 0.081 Uiso 1 calc R . . H14B H 0.1719 0.8681 0.0395 0.081 Uiso 1 calc R . . H14C H 0.0586 0.8755 0.0903 0.081 Uiso 1 calc R . . C15 C 0.2323(5) 1.0039(4) 0.1433(4) 0.0590(14) Uani 1 d . . . H15A H 0.1558 1.0379 0.1418 0.088 Uiso 1 calc R . . H15B H 0.2755 1.0196 0.0986 0.088 Uiso 1 calc R . . H15C H 0.2766 1.0290 0.1853 0.088 Uiso 1 calc R . . C16 C 0.3370(5) 0.8284(5) 0.1471(3) 0.0539(14) Uani 1 d . . . H16A H 0.3875 0.8554 0.1857 0.081 Uiso 1 calc R . . H16B H 0.3737 0.8406 0.0997 0.081 Uiso 1 calc R . . H16C H 0.3255 0.7543 0.1542 0.081 Uiso 1 calc R . . N' N 0.2965(4) 0.9570(3) 0.7860(2) 0.0473(10) Uani 1 d D . . H0' H 0.334(3) 1.0177(12) 0.7939(8) 0.057 Uiso 1 d D . . C1' C 0.1910(5) 0.8142(4) 0.5942(3) 0.0477(12) Uani 1 d . . . H1' H 0.1439 0.7420 0.5777 0.057 Uiso 1 calc R . . B3' B 0.3412(5) 0.8297(4) 0.5796(3) 0.0395(13) Uani 1 d . . . H3' H 0.3965 0.7687 0.5534 0.047 Uiso 1 calc R . . B4' B 0.2898(7) 0.8089(5) 0.6709(4) 0.0434(16) Uani 1 d . . . H4' H 0.3087 0.7375 0.7032 0.052 Uiso 1 calc R . . B5' B 0.1492(5) 0.8748(5) 0.6764(3) 0.0433(14) Uani 1 d . . . H5' H 0.0765 0.8459 0.7121 0.052 Uiso 1 calc R . . B6' B 0.1250(5) 0.9338(4) 0.5910(3) 0.0379(12) Uani 1 d . . . H6' H 0.0323 0.9442 0.5722 0.046 Uiso 1 calc R . . C7' C 0.3669(4) 0.9619(4) 0.5662(3) 0.0493(12) Uani 1 d . . . H7' H 0.4398 0.9916 0.5311 0.059 Uiso 1 calc R . . B8' B 0.4012(5) 0.9025(4) 0.6528(3) 0.0417(12) Uani 1 d . . . H8' H 0.4932 0.8920 0.6729 0.050 Uiso 1 calc R . . C9' C 0.2810(5) 0.9318(4) 0.7091(3) 0.0381(11) Uani 1 d D . . B10' B 0.1775(6) 1.0085(5) 0.6638(3) 0.0431(15) Uani 1 d . . . H10' H 0.1227 1.0680 0.6922 0.052 Uiso 1 calc R . . B11' B 0.2307(5) 1.0273(4) 0.5747(3) 0.0415(12) Uani 1 d . . . H11' H 0.2110 1.1016 0.5460 0.050 Uiso 1 calc R . . B12' B 0.3314(5) 1.0270(4) 0.6495(3) 0.0439(12) Uani 1 d . . . H12' H 0.3785 1.0981 0.6681 0.053 Uiso 1 calc R . . C13' C 0.3197(5) 0.8841(4) 0.8481(3) 0.0433(11) Uani 1 d D . . C14' C 0.3326(6) 0.9556(5) 0.9153(3) 0.0619(15) Uani 1 d . . . H14D H 0.3954 1.0055 0.9064 0.093 Uiso 1 calc R . . H14E H 0.3518 0.9142 0.9582 0.093 Uiso 1 calc R . . H14F H 0.2589 0.9923 0.9236 0.093 Uiso 1 calc R . . C15' C 0.4366(5) 0.8241(4) 0.8377(3) 0.0644(15) Uani 1 d . . . H15D H 0.4274 0.7734 0.7987 0.097 Uiso 1 calc R . . H15E H 0.4569 0.7886 0.8831 0.097 Uiso 1 calc R . . H15F H 0.4991 0.8724 0.8250 0.097 Uiso 1 calc R . . C16' C 0.2137(5) 0.8103(5) 0.8603(3) 0.0600(15) Uani 1 d . . . H16D H 0.1450 0.8505 0.8748 0.090 Uiso 1 calc R . . H16E H 0.2329 0.7608 0.8987 0.090 Uiso 1 calc R . . H16F H 0.1967 0.7732 0.8151 0.090 Uiso 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 N 0.0361(19) 0.051(2) 0.039(2) -0.0040(18) -0.0018(17) -0.0075(18) C1 0.034(2) 0.050(3) 0.047(3) -0.008(2) 0.002(2) -0.006(2) Fe2 0.0295(3) 0.0285(3) 0.0380(3) -0.0032(3) 0.0027(4) -0.0010(2) B3 0.037(3) 0.040(3) 0.042(3) -0.005(2) 0.001(2) 0.009(2) B4 0.033(3) 0.054(3) 0.047(3) -0.007(3) 0.001(2) 0.005(2) B5 0.043(3) 0.033(3) 0.051(3) -0.001(2) -0.002(2) -0.009(2) B6 0.047(3) 0.029(3) 0.040(3) -0.004(2) -0.001(2) -0.002(2) C7 0.044(3) 0.039(3) 0.052(3) 0.000(2) 0.002(2) -0.005(2) B8 0.047(4) 0.036(3) 0.044(3) -0.003(3) 0.003(3) 0.002(3) C9 0.033(2) 0.034(2) 0.041(2) 0.000(2) 0.001(2) 0.000(2) B10 0.035(3) 0.036(3) 0.044(4) -0.006(3) 0.000(2) 0.005(2) B11 0.028(3) 0.035(3) 0.040(3) -0.007(2) 0.004(2) -0.001(2) B12 0.033(3) 0.042(3) 0.045(3) -0.007(3) 0.009(3) -0.007(2) C13 0.050(3) 0.041(3) 0.038(2) 0.001(2) 0.004(2) -0.003(2) C14 0.062(3) 0.054(3) 0.046(3) 0.001(3) -0.003(3) 0.001(3) C15 0.072(4) 0.045(3) 0.060(3) 0.004(3) -0.004(3) -0.007(3) C16 0.051(3) 0.065(3) 0.046(3) -0.007(3) 0.009(2) 0.005(3) N' 0.063(3) 0.036(2) 0.042(2) -0.0069(19) 0.001(2) -0.0091(19) C1' 0.050(3) 0.042(3) 0.052(3) 0.000(2) 0.007(2) -0.006(2) B3' 0.040(3) 0.034(3) 0.044(3) -0.005(2) -0.003(2) 0.004(2) B4' 0.056(4) 0.033(3) 0.042(4) -0.002(3) 0.002(3) 0.000(3) B5' 0.036(3) 0.050(3) 0.044(3) 0.001(3) 0.006(2) -0.010(3) B6' 0.034(3) 0.043(3) 0.037(3) -0.002(3) 0.006(2) 0.003(2) C7' 0.042(3) 0.058(3) 0.048(3) -0.004(3) 0.005(2) -0.006(2) B8' 0.036(3) 0.047(3) 0.042(3) -0.004(3) 0.002(2) 0.005(2) C9' 0.038(3) 0.033(2) 0.042(3) -0.003(2) 0.004(2) -0.0059(19) B10' 0.047(4) 0.035(3) 0.047(3) -0.004(3) 0.006(3) 0.007(3) B11' 0.047(3) 0.030(3) 0.047(3) -0.007(3) 0.002(2) 0.001(2) B12' 0.056(3) 0.035(3) 0.040(3) -0.005(2) 0.004(3) -0.011(2) C13' 0.047(3) 0.039(3) 0.044(3) 0.001(2) -0.003(2) -0.004(2) C14' 0.086(4) 0.058(3) 0.042(3) -0.002(3) -0.003(3) -0.016(3) C15' 0.058(3) 0.068(3) 0.067(4) 0.003(3) -0.009(3) 0.010(3) C16' 0.064(3) 0.063(4) 0.054(3) 0.000(3) 0.007(3) -0.017(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 N C9 1.423(6) . ? N C13 1.477(6) . ? N H0 0.8899(11) . ? C1 B3 1.696(7) . ? C1 B4 1.719(7) . ? C1 B5 1.720(7) . ? C1 B6 1.720(7) . ? C1 Fe2 2.067(5) . ? C1 H1 1.1000 . ? Fe2 B3 2.047(5) . ? Fe2 C7 2.052(5) . ? Fe2 B6 2.053(5) . ? Fe2 B11 2.061(6) . ? Fe2 B6' 2.069(5) . ? Fe2 C7' 2.074(5) . ? Fe2 C1' 2.079(5) . ? Fe2 B11' 2.090(6) . ? Fe2 B3' 2.096(6) . ? B3 C7 1.722(7) . ? B3 B4 1.758(8) . ? B3 B8 1.778(8) . ? B3 H3 1.1000 . ? B4 C9 1.704(7) . ? B4 B8 1.736(8) . ? B4 B5 1.779(7) . ? B4 H4 1.1000 . ? B5 C9 1.701(7) . ? B5 B10 1.751(8) . ? B5 B6 1.788(7) . ? B5 H5 1.1000 . ? B6 B11 1.722(7) . ? B6 B10 1.785(8) . ? B6 H6 1.1000 . ? C7 B11 1.723(7) . ? C7 B8 1.751(8) . ? C7 B12 1.773(7) . ? C7 H7 1.1000 . ? B8 C9 1.752(7) . ? B8 B12 1.790(9) . ? B8 H8 1.1000 . ? C9 B10 1.727(8) . ? C9 B12 1.728(7) . ? B10 B11 1.736(8) . ? B10 B12 1.759(8) . ? B10 H10 1.1000 . ? B11 B12 1.745(8) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C13 C14 1.526(7) . ? C13 C15 1.534(7) . ? C13 C16 1.544(7) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? N' C9' 1.431(6) . ? N' C13' 1.477(6) . ? N' H0' 0.8900(11) . ? C1' B6' 1.693(7) . ? C1' B3' 1.714(8) . ? C1' B5' 1.734(8) . ? C1' B4' 1.771(9) . ? C1' H1' 1.1000 . ? B3' C7' 1.724(8) . ? B3' B8' 1.746(8) . ? B3' B4' 1.763(9) . ? B3' H3' 1.1000 . ? B4' C9' 1.712(8) . ? B4' B8' 1.756(9) . ? B4' B5' 1.786(10) . ? B4' H4' 1.1000 . ? B5' B6' 1.735(8) . ? B5' B10' 1.746(9) . ? B5' C9' 1.747(8) . ? B5' H5' 1.1000 . ? B6' B11' 1.703(8) . ? B6' B10' 1.724(8) . ? B6' H6' 1.1000 . ? C7' B11' 1.745(7) . ? C7' B12' 1.759(7) . ? C7' B8' 1.775(8) . ? C7' H7' 1.1000 . ? B8' C9' 1.727(7) . ? B8' B12' 1.767(7) . ? B8' H8' 1.1000 . ? C9' B12' 1.714(7) . ? C9' B10' 1.721(8) . ? B10' B11' 1.729(9) . ? B10' B12' 1.758(9) . ? B10' H10' 1.1000 . ? B11' B12' 1.758(8) . ? B11' H11' 1.1000 . ? B12' H12' 1.1000 . ? C13' C14' 1.521(7) . ? C13' C15' 1.528(7) . ? C13' C16' 1.529(7) . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15' H15D 0.9600 . ? C15' H15E 0.9600 . ? C15' H15F 0.9600 . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? 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 C9 N C13 128.6(4) . . ? C9 N H0 115.0(10) . . ? C13 N H0 109.8(10) . . ? B3 C1 B4 62.0(3) . . ? B3 C1 B5 112.7(4) . . ? B4 C1 B5 62.3(3) . . ? B3 C1 B6 110.9(3) . . ? B4 C1 B6 112.8(4) . . ? B5 C1 B6 62.6(3) . . ? B3 C1 Fe2 65.0(2) . . ? B4 C1 Fe2 120.8(3) . . ? B5 C1 Fe2 121.3(3) . . ? B6 C1 Fe2 64.9(2) . . ? B3 C1 H1 120.4 . . ? B4 C1 H1 117.1 . . ? B5 C1 H1 116.7 . . ? B6 C1 H1 120.1 . . ? Fe2 C1 H1 111.0 . . ? B3 Fe2 C7 49.7(2) . . ? B3 Fe2 B6 86.7(2) . . ? C7 Fe2 B6 86.1(2) . . ? B3 Fe2 B11 85.4(2) . . ? C7 Fe2 B11 49.5(2) . . ? B6 Fe2 B11 49.5(2) . . ? B3 Fe2 C1 48.7(2) . . ? C7 Fe2 C1 83.32(19) . . ? B6 Fe2 C1 49.35(19) . . ? B11 Fe2 C1 83.0(2) . . ? B3 Fe2 B6' 94.8(2) . . ? C7 Fe2 B6' 131.1(2) . . ? B6 Fe2 B6' 129.7(2) . . ? B11 Fe2 B6' 179.2(2) . . ? C1 Fe2 B6' 96.5(2) . . ? B3 Fe2 C7' 130.0(2) . . ? C7 Fe2 C7' 95.4(2) . . ? B6 Fe2 C7' 131.3(2) . . ? B11 Fe2 C7' 96.6(2) . . ? C1 Fe2 C7' 178.6(2) . . ? B6' Fe2 C7' 83.9(2) . . ? B3 Fe2 C1' 130.6(2) . . ? C7 Fe2 C1' 178.8(2) . . ? B6 Fe2 C1' 95.0(2) . . ? B11 Fe2 C1' 131.2(2) . . ? C1 Fe2 C1' 97.6(2) . . ? B6' Fe2 C1' 48.2(2) . . ? C7' Fe2 C1' 83.6(2) . . ? B3 Fe2 B11' 93.7(2) . . ? C7 Fe2 B11' 95.6(2) . . ? B6 Fe2 B11' 178.0(2) . . ? B11 Fe2 B11' 132.4(2) . . ? C1 Fe2 B11' 129.9(2) . . ? B6' Fe2 B11' 48.3(2) . . ? C7' Fe2 B11' 49.6(2) . . ? C1' Fe2 B11' 83.3(2) . . ? B3 Fe2 B3' 177.7(2) . . ? C7 Fe2 B3' 131.2(2) . . ? B6 Fe2 B3' 95.4(2) . . ? B11 Fe2 B3' 96.6(2) . . ? C1 Fe2 B3' 132.5(2) . . ? B6' Fe2 B3' 83.3(2) . . ? C7' Fe2 B3' 48.8(2) . . ? C1' Fe2 B3' 48.5(2) . . ? B11' Fe2 B3' 84.1(2) . . ? C1 B3 C7 106.5(4) . . ? C1 B3 B4 59.7(3) . . ? C7 B3 B4 106.7(4) . . ? C1 B3 B8 106.4(4) . . ? C7 B3 B8 60.0(3) . . ? B4 B3 B8 58.8(3) . . ? C1 B3 Fe2 66.3(2) . . ? C7 B3 Fe2 65.3(2) . . ? B4 B3 Fe2 119.9(3) . . ? B8 B3 Fe2 119.5(3) . . ? C1 B3 H3 123.2 . . ? C7 B3 H3 123.4 . . ? B4 B3 H3 120.3 . . ? B8 B3 H3 120.5 . . ? Fe2 B3 H3 109.8 . . ? C9 B4 C1 104.1(4) . . ? C9 B4 B8 61.2(3) . . ? C1 B4 B8 107.2(4) . . ? C9 B4 B3 107.5(4) . . ? C1 B4 B3 58.4(3) . . ? B8 B4 B3 61.2(3) . . ? C9 B4 B5 58.4(3) . . ? C1 B4 B5 58.9(3) . . ? B8 B4 B5 109.1(4) . . ? B3 B4 B5 107.1(4) . . ? C9 B4 H4 123.2 . . ? C1 B4 H4 124.2 . . ? B8 B4 H4 120.1 . . ? B3 B4 H4 121.9 . . ? B5 B4 H4 122.1 . . ? C9 B5 C1 104.2(3) . . ? C9 B5 B10 60.0(3) . . ? C1 B5 B10 106.4(4) . . ? C9 B5 B4 58.6(3) . . ? C1 B5 B4 58.8(3) . . ? B10 B5 B4 107.7(4) . . ? C9 B5 B6 106.9(3) . . ? C1 B5 B6 58.7(3) . . ? B10 B5 B6 60.6(3) . . ? B4 B5 B6 106.9(4) . . ? C9 B5 H5 123.4 . . ? C1 B5 H5 124.0 . . ? B10 B5 H5 121.4 . . ? B4 B5 H5 122.4 . . ? B6 B5 H5 122.0 . . ? C1 B6 B11 105.3(4) . . ? C1 B6 B10 104.9(4) . . ? B11 B6 B10 59.3(3) . . ? C1 B6 B5 58.7(3) . . ? B11 B6 B5 105.7(4) . . ? B10 B6 B5 58.7(3) . . ? C1 B6 Fe2 65.8(2) . . ? B11 B6 Fe2 65.5(2) . . ? B10 B6 Fe2 118.7(3) . . ? B5 B6 Fe2 118.6(3) . . ? C1 B6 H6 124.3 . . ? B11 B6 H6 123.8 . . ? B10 B6 H6 121.1 . . ? B5 B6 H6 121.1 . . ? Fe2 B6 H6 110.3 . . ? B3 C7 B11 108.0(4) . . ? B3 C7 B8 61.6(3) . . ? B11 C7 B8 108.9(4) . . ? B3 C7 B12 110.0(4) . . ? B11 C7 B12 59.9(3) . . ? B8 C7 B12 61.0(3) . . ? B3 C7 Fe2 65.0(3) . . ? B11 C7 Fe2 65.5(3) . . ? B8 C7 Fe2 120.6(3) . . ? B12 C7 Fe2 119.8(3) . . ? B3 C7 H7 121.7 . . ? B11 C7 H7 122.7 . . ? B8 C7 H7 118.3 . . ? B12 C7 H7 118.9 . . ? Fe2 C7 H7 110.5 . . ? B4 B8 C7 106.3(4) . . ? B4 B8 C9 58.5(3) . . ? C7 B8 C9 104.4(4) . . ? B4 B8 B3 60.0(3) . . ? C7 B8 B3 58.4(3) . . ? C9 B8 B3 104.6(4) . . ? B4 B8 B12 106.8(4) . . ? C7 B8 B12 60.1(3) . . ? C9 B8 B12 58.4(3) . . ? B3 B8 B12 106.7(4) . . ? B4 B8 H8 122.2 . . ? C7 B8 H8 123.2 . . ? C9 B8 H8 124.6 . . ? B3 B8 H8 123.0 . . ? B12 B8 H8 122.1 . . ? N C9 B5 113.8(4) . . ? N C9 B4 115.1(4) . . ? B5 C9 B4 63.0(3) . . ? N C9 B10 120.5(4) . . ? B5 C9 B10 61.4(3) . . ? B4 C9 B10 112.3(4) . . ? N C9 B12 125.6(4) . . ? B5 C9 B12 111.7(4) . . ? B4 C9 B12 111.2(4) . . ? B10 C9 B12 61.2(3) . . ? N C9 B8 122.0(4) . . ? B5 C9 B8 112.1(4) . . ? B4 C9 B8 60.3(3) . . ? B10 C9 B8 111.7(4) . . ? B12 C9 B8 61.9(3) . . ? C9 B10 B11 105.0(4) . . ? C9 B10 B5 58.5(3) . . ? B11 B10 B5 106.7(4) . . ? C9 B10 B12 59.4(3) . . ? B11 B10 B12 59.9(3) . . ? B5 B10 B12 107.8(4) . . ? C9 B10 B6 105.8(4) . . ? B11 B10 B6 58.5(3) . . ? B5 B10 B6 60.7(3) . . ? B12 B10 B6 107.6(4) . . ? C9 B10 H10 123.9 . . ? B11 B10 H10 123.3 . . ? B5 B10 H10 121.8 . . ? B12 B10 H10 121.4 . . ? B6 B10 H10 122.3 . . ? B6 B11 C7 109.0(4) . . ? B6 B11 B10 62.2(3) . . ? C7 B11 B10 109.8(4) . . ? B6 B11 B12 111.2(4) . . ? C7 B11 B12 61.5(3) . . ? B10 B11 B12 60.7(3) . . ? B6 B11 Fe2 65.0(3) . . ? C7 B11 Fe2 65.0(3) . . ? B10 B11 Fe2 120.8(4) . . ? B12 B11 Fe2 120.7(3) . . ? B6 B11 H11 121.0 . . ? C7 B11 H11 121.9 . . ? B10 B11 H11 118.2 . . ? B12 B11 H11 117.9 . . ? Fe2 B11 H11 110.6 . . ? C9 B12 B11 104.5(4) . . ? C9 B12 B10 59.4(3) . . ? B11 B12 B10 59.4(3) . . ? C9 B12 C7 104.5(4) . . ? B11 B12 C7 58.6(3) . . ? B10 B12 C7 106.5(4) . . ? C9 B12 B8 59.7(3) . . ? B11 B12 B8 106.2(4) . . ? B10 B12 B8 108.5(4) . . ? C7 B12 B8 58.9(3) . . ? C9 B12 H12 123.9 . . ? B11 B12 H12 123.6 . . ? B10 B12 H12 121.5 . . ? C7 B12 H12 123.7 . . ? B8 B12 H12 121.7 . . ? N C13 C14 104.7(4) . . ? N C13 C15 111.8(4) . . ? C14 C13 C15 109.4(4) . . ? N C13 C16 111.3(4) . . ? C14 C13 C16 109.3(4) . . ? C15 C13 C16 110.1(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C9' N' C13' 127.9(4) . . ? C9' N' H0' 113.9(10) . . ? C13' N' H0' 110.0(10) . . ? B6' C1' B3' 108.6(4) . . ? B6' C1' B5' 60.8(3) . . ? B3' C1' B5' 110.2(4) . . ? B6' C1' B4' 109.5(4) . . ? B3' C1' B4' 60.7(3) . . ? B5' C1' B4' 61.2(4) . . ? B6' C1' Fe2 65.6(3) . . ? B3' C1' Fe2 66.3(3) . . ? B5' C1' Fe2 121.2(3) . . ? B4' C1' Fe2 121.3(3) . . ? B6' C1' H1' 122.2 . . ? B3' C1' H1' 121.6 . . ? B5' C1' H1' 118.2 . . ? B4' C1' H1' 118.5 . . ? Fe2 C1' H1' 109.4 . . ? C1' B3' C7' 107.3(4) . . ? C1' B3' B8' 108.8(4) . . ? C7' B3' B8' 61.5(3) . . ? C1' B3' B4' 61.3(4) . . ? C7' B3' B4' 109.3(4) . . ? B8' B3' B4' 60.0(4) . . ? C1' B3' Fe2 65.3(3) . . ? C7' B3' Fe2 64.9(3) . . ? B8' B3' Fe2 120.6(3) . . ? B4' B3' Fe2 120.9(4) . . ? C1' B3' H3' 122.5 . . ? C7' B3' H3' 122.4 . . ? B8' B3' H3' 118.8 . . ? B4' B3' H3' 118.6 . . ? Fe2 B3' H3' 110.2 . . ? C9' B4' B8' 59.7(3) . . ? C9' B4' B3' 104.9(4) . . ? B8' B4' B3' 59.5(3) . . ? C9' B4' C1' 104.1(4) . . ? B8' B4' C1' 105.9(4) . . ? B3' B4' C1' 58.0(3) . . ? C9' B4' B5' 59.9(3) . . ? B8' B4' B5' 108.6(5) . . ? B3' B4' B5' 105.6(4) . . ? C1' B4' B5' 58.4(3) . . ? C9' B4' H4' 123.6 . . ? B8' B4' H4' 121.4 . . ? B3' B4' H4' 123.7 . . ? C1' B4' H4' 124.4 . . ? B5' B4' H4' 121.9 . . ? C1' B5' B6' 58.4(3) . . ? C1' B5' B10' 105.8(4) . . ? B6' B5' B10' 59.4(3) . . ? C1' B5' C9' 104.2(4) . . ? B6' B5' C9' 104.5(4) . . ? B10' B5' C9' 59.0(4) . . ? C1' B5' B4' 60.4(3) . . ? B6' B5' B4' 106.9(4) . . ? B10' B5' B4' 106.9(5) . . ? C9' B5' B4' 58.0(3) . . ? C1' B5' H5' 123.3 . . ? B6' B5' H5' 123.1 . . ? B10' B5' H5' 122.4 . . ? C9' B5' H5' 124.6 . . ? B4' B5' H5' 121.9 . . ? C1' B6' B11' 109.3(4) . . ? C1' B6' B10' 108.7(4) . . ? B11' B6' B10' 60.6(3) . . ? C1' B6' B5' 60.8(3) . . ? B11' B6' B5' 110.3(4) . . ? B10' B6' B5' 60.6(4) . . ? C1' B6' Fe2 66.2(3) . . ? B11' B6' Fe2 66.5(3) . . ? B10' B6' Fe2 121.0(4) . . ? B5' B6' Fe2 121.8(4) . . ? C1' B6' H6' 122.0 . . ? B11' B6' H6' 121.3 . . ? B10' B6' H6' 119.3 . . ? B5' B6' H6' 118.2 . . ? Fe2 B6' H6' 109.0 . . ? B3' C7' B11' 107.9(4) . . ? B3' C7' B12' 107.6(4) . . ? B11' C7' B12' 60.2(3) . . ? B3' C7' B8' 59.9(3) . . ? B11' C7' B8' 108.4(4) . . ? B12' C7' B8' 60.0(3) . . ? B3' C7' Fe2 66.2(3) . . ? B11' C7' Fe2 65.7(2) . . ? B12' C7' Fe2 120.0(3) . . ? B8' C7' Fe2 120.4(3) . . ? B3' C7' H7' 122.6 . . ? B11' C7' H7' 122.4 . . ? B12' C7' H7' 119.8 . . ? B8' C7' H7' 119.5 . . ? Fe2 C7' H7' 109.7 . . ? C9' B8' B3' 105.0(4) . . ? C9' B8' B4' 58.9(3) . . ? B3' B8' B4' 60.4(3) . . ? C9' B8' B12' 58.7(3) . . ? B3' B8' B12' 106.3(4) . . ? B4' B8' B12' 107.4(4) . . ? C9' B8' C7' 104.8(4) . . ? B3' B8' C7' 58.6(3) . . ? B4' B8' C7' 107.4(4) . . ? B12' B8' C7' 59.6(3) . . ? C9' B8' H8' 124.2 . . ? B3' B8' H8' 123.0 . . ? B4' B8' H8' 121.4 . . ? B12' B8' H8' 122.3 . . ? C7' B8' H8' 123.0 . . ? N' C9' B4' 125.9(4) . . ? N' C9' B12' 114.1(4) . . ? B4' C9' B12' 112.0(4) . . ? N' C9' B10' 114.4(4) . . ? B4' C9' B10' 111.5(4) . . ? B12' C9' B10' 61.6(4) . . ? N' C9' B8' 121.5(4) . . ? B4' C9' B8' 61.4(3) . . ? B12' C9' B8' 61.8(3) . . ? B10' C9' B8' 111.6(4) . . ? N' C9' B5' 121.4(4) . . ? B4' C9' B5' 62.1(4) . . ? B12' C9' B5' 111.1(4) . . ? B10' C9' B5' 60.5(3) . . ? B8' C9' B5' 111.7(4) . . ? C9' B10' B6' 106.1(4) . . ? C9' B10' B11' 106.7(4) . . ? B6' B10' B11' 59.1(3) . . ? C9' B10' B5' 60.5(3) . . ? B6' B10' B5' 60.0(3) . . ? B11' B10' B5' 108.5(4) . . ? C9' B10' B12' 59.0(3) . . ? B6' B10' B12' 107.2(4) . . ? B11' B10' B12' 60.5(3) . . ? B5' B10' B12' 109.1(4) . . ? C9' B10' H10' 123.0 . . ? B6' B10' H10' 122.9 . . ? B11' B10' H10' 121.9 . . ? B5' B10' H10' 120.6 . . ? B12' B10' H10' 121.5 . . ? B6' B11' B10' 60.3(3) . . ? B6' B11' C7' 106.8(4) . . ? B10' B11' C7' 108.4(4) . . ? B6' B11' B12' 108.2(4) . . ? B10' B11' B12' 60.6(4) . . ? C7' B11' B12' 60.3(3) . . ? B6' B11' Fe2 65.2(3) . . ? B10' B11' Fe2 119.6(4) . . ? C7' B11' Fe2 64.7(2) . . ? B12' B11' Fe2 119.2(3) . . ? B6' B11' H11' 122.9 . . ? B10' B11' H11' 119.1 . . ? C7' B11' H11' 123.0 . . ? B12' B11' H11' 119.4 . . ? Fe2 B11' H11' 110.9 . . ? C9' B12' B11' 105.7(4) . . ? C9' B12' B10' 59.4(3) . . ? B11' B12' B10' 58.9(3) . . ? C9' B12' C7' 106.0(4) . . ? B11' B12' C7' 59.5(3) . . ? B10' B12' C7' 106.5(4) . . ? C9' B12' B8' 59.5(3) . . ? B11' B12' B8' 108.2(4) . . ? B10' B12' B8' 108.0(4) . . ? C7' B12' B8' 60.4(3) . . ? C9' B12' H12' 123.3 . . ? B11' B12' H12' 122.6 . . ? B10' B12' H12' 122.4 . . ? C7' B12' H12' 122.6 . . ? B8' B12' H12' 121.1 . . ? N' C13' C14' 104.1(4) . . ? N' C13' C15' 111.9(4) . . ? C14' C13' C15' 108.3(5) . . ? N' C13' C16' 111.0(5) . . ? C14' C13' C16' 109.1(5) . . ? C15' C13' C16' 112.0(5) . . ? C13' C14' H14D 109.5 . . ? C13' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C13' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? C13' C15' H15D 109.5 . . ? C13' C15' H15E 109.5 . . ? H15D C15' H15E 109.5 . . ? C13' C15' H15F 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? C13' C16' H16D 109.5 . . ? C13' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C13' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.255 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.047 #===END data_compound_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C14 H40 B16 N2 Ru' _chemical_formula_sum 'C14 H40 B16 N2 Ru' _chemical_formula_weight 510.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 2(1) 2(1) 2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.846(2) _cell_length_b 19.816(2) _cell_length_c 11.089(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2603.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17.47 _cell_measurement_theta_max 20.58 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.610 _exptl_absorpt_correction_type 'psi-scan (North, Phillips & Mathews 1968)' _exptl_absorpt_correction_T_min 0.8287 _exptl_absorpt_correction_T_max 0.8981 _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method '\w--2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 2608 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2608 _reflns_number_gt 2335 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; MSC/AFC5S Control Program (Molecular Structure Corporation, 1995) ; _computing_cell_refinement ; MSC/AFC5S Control Program (Molecular Structure Corporation, 1995) ; _computing_data_reduction ; TEXSAN (Molecular Structure Corporation, 1989) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP II (Johnson, 1976)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _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 w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.5601P] 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 -0.13(5) _refine_ls_number_reflns 2608 _refine_ls_number_parameters 310 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.040 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N N -0.1475(3) 1.0013(2) 0.1255(4) 0.0442(10) Uani 1 d D . . H0 H -0.1982(9) 0.9739(10) 0.092(3) 0.053 Uiso 1 d D . . C1 C 0.1826(4) 0.9805(3) 0.2082(5) 0.0443(13) Uani 1 d . . . H1 H 0.2492 1.0139 0.2431 0.053 Uiso 1 calc R . . Ru2 Ru 0.25539(3) 0.880911(15) 0.17587(3) 0.02921(12) Uani 1 d . . . B3 B 0.1808(5) 0.9552(3) 0.0571(5) 0.0402(14) Uani 1 d . . . H3 H 0.2451 0.9689 -0.0101 0.048 Uiso 1 calc R . . B4 B 0.0824(5) 1.0156(3) 0.1142(6) 0.0384(13) Uani 1 d . . . H4 H 0.0843 1.0687 0.0850 0.046 Uiso 1 calc R . . B5 B 0.0472(5) 0.9920(3) 0.2641(5) 0.0397(13) Uani 1 d . . . H5 H 0.0255 1.0297 0.3331 0.048 Uiso 1 calc R . . B6 B 0.1241(5) 0.9186(3) 0.2959(5) 0.0331(12) Uani 1 d . . . H6 H 0.1509 0.9096 0.3894 0.040 Uiso 1 calc R . . C7 C 0.1056(4) 0.8804(3) 0.0573(5) 0.0403(13) Uani 1 d . . . H7 H 0.1179 0.8433 -0.0154 0.048 Uiso 1 calc R . . B8 B 0.0353(5) 0.9522(3) 0.0184(6) 0.0426(13) Uani 1 d . . . H8 H 0.0063 0.9640 -0.0735 0.051 Uiso 1 calc R . . C9 C -0.0404(4) 0.9721(2) 0.1479(4) 0.0368(11) Uani 1 d D . . B10 B -0.0188(5) 0.9122(3) 0.2606(5) 0.0380(13) Uani 1 d . . . H10 H -0.0830 0.8975 0.3273 0.046 Uiso 1 calc R . . B11 B 0.0795(5) 0.8516(3) 0.2010(6) 0.0410(13) Uani 1 d . . . H11 H 0.0769 0.7981 0.2275 0.049 Uiso 1 calc R . . B12 B -0.0287(5) 0.8877(3) 0.1076(6) 0.0403(14) Uani 1 d . . . H12 H -0.1000 0.8575 0.0741 0.048 Uiso 1 calc R . . C13 C -0.2044(4) 1.0550(3) 0.1952(5) 0.0441(12) Uani 1 d D . . C14 C -0.3144(5) 1.0677(3) 0.1277(6) 0.0650(18) Uani 1 d . . . H14A H -0.2979 1.0813 0.0465 0.098 Uiso 1 calc R . . H14B H -0.3561 1.1027 0.1675 0.098 Uiso 1 calc R . . H14C H -0.3585 1.0270 0.1265 0.098 Uiso 1 calc R . . C15 C -0.2340(5) 1.0311(3) 0.3235(5) 0.0672(16) Uani 1 d . . . H15A H -0.2756 0.9896 0.3191 0.101 Uiso 1 calc R . . H15B H -0.2791 1.0648 0.3629 0.101 Uiso 1 calc R . . H15C H -0.1658 1.0241 0.3685 0.101 Uiso 1 calc R . . C16 C -0.1358(5) 1.1198(3) 0.1989(6) 0.0652(17) Uani 1 d . . . H16A H -0.0677 1.1124 0.2439 0.098 Uiso 1 calc R . . H16B H -0.1793 1.1547 0.2370 0.098 Uiso 1 calc R . . H16C H -0.1171 1.1333 0.1182 0.098 Uiso 1 calc R . . N' N 0.6584(3) 0.7578(2) 0.2048(4) 0.0446(11) Uani 1 d D . . H0' H 0.7116(8) 0.7811(12) 0.166(2) 0.053 Uiso 1 d D . . C1' C 0.3255(4) 0.7878(2) 0.2534(4) 0.0373(12) Uani 1 d . . . H1' H 0.2574 0.7585 0.2959 0.045 Uiso 1 calc R . . B3' B 0.3361(5) 0.7934(3) 0.0969(5) 0.0354(12) Uani 1 d . . . H3' H 0.2760 0.7711 0.0328 0.042 Uiso 1 calc R . . B4' B 0.4312(4) 0.7425(3) 0.1843(5) 0.0361(12) Uani 1 d . . . H4' H 0.4312 0.6872 0.1774 0.043 Uiso 1 calc R . . B5' B 0.4554(5) 0.7854(3) 0.3222(5) 0.0375(12) Uani 1 d . . . H5' H 0.4720 0.7578 0.4065 0.045 Uiso 1 calc R . . B6' B 0.3760(4) 0.8609(3) 0.3181(5) 0.0343(12) Uani 1 d . . . H6' H 0.3416 0.8818 0.4023 0.041 Uiso 1 calc R . . C7' C 0.4121(4) 0.8671(3) 0.0719(5) 0.0378(13) Uani 1 d . . . H7' H 0.4047 0.8936 -0.0148 0.045 Uiso 1 calc R . . B8' B 0.4851(5) 0.7926(3) 0.0699(5) 0.0382(13) Uani 1 d . . . H8' H 0.5205 0.7699 -0.0124 0.046 Uiso 1 calc R . . C9' C 0.5508(4) 0.7899(2) 0.2078(4) 0.0346(11) Uani 1 d D . . B10' B 0.5226(5) 0.8638(3) 0.2926(5) 0.0400(14) Uani 1 d . . . H10' H 0.5819 0.8874 0.3563 0.048 Uiso 1 calc R . . B11' B 0.4299(4) 0.9132(3) 0.2030(6) 0.0406(14) Uani 1 d . . . H11' H 0.4321 0.9686 0.2073 0.049 Uiso 1 calc R . . B12' B 0.5436(5) 0.8668(3) 0.1362(6) 0.0398(15) Uani 1 d . . . H12' H 0.6178 0.8922 0.0977 0.048 Uiso 1 calc R . . C13' C 0.7111(4) 0.7191(3) 0.3050(5) 0.0436(12) Uani 1 d D . . C14' C 0.8282(5) 0.6995(4) 0.2540(6) 0.0668(19) Uani 1 d . . . H14D H 0.8186 0.6694 0.1869 0.100 Uiso 1 calc R . . H14E H 0.8716 0.6775 0.3157 0.100 Uiso 1 calc R . . H14F H 0.8671 0.7393 0.2277 0.100 Uiso 1 calc R . . C15' C 0.6453(5) 0.6537(3) 0.3298(6) 0.0612(16) Uani 1 d . . . H15D H 0.5739 0.6645 0.3659 0.092 Uiso 1 calc R . . H15E H 0.6880 0.6256 0.3836 0.092 Uiso 1 calc R . . H15F H 0.6330 0.6302 0.2553 0.092 Uiso 1 calc R . . C16' C 0.7291(5) 0.7599(4) 0.4194(5) 0.0715(18) Uani 1 d . . . H16D H 0.7634 0.8023 0.3995 0.107 Uiso 1 calc R . . H16E H 0.7777 0.7353 0.4731 0.107 Uiso 1 calc R . . H16F H 0.6577 0.7677 0.4579 0.107 Uiso 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 N 0.033(2) 0.052(3) 0.047(3) -0.011(2) -0.004(2) 0.0062(19) C1 0.049(3) 0.036(3) 0.048(3) -0.005(2) -0.001(3) -0.002(2) Ru2 0.03022(18) 0.02874(18) 0.02869(18) -0.00033(13) -0.00035(19) -0.00197(17) B3 0.041(3) 0.047(3) 0.033(3) 0.012(3) 0.003(3) 0.009(3) B4 0.040(3) 0.031(3) 0.044(3) 0.006(3) 0.003(3) -0.001(2) B5 0.042(3) 0.037(3) 0.040(3) -0.006(3) 0.001(3) 0.006(3) B6 0.037(3) 0.030(3) 0.032(3) -0.002(2) 0.003(2) 0.002(2) C7 0.034(2) 0.045(3) 0.042(3) -0.009(3) -0.007(2) 0.012(3) B8 0.037(3) 0.056(4) 0.034(3) -0.001(3) -0.001(3) 0.007(3) C9 0.037(2) 0.036(3) 0.038(3) -0.002(2) 0.004(2) 0.000(2) B10 0.041(3) 0.037(3) 0.036(3) 0.009(3) 0.007(3) 0.002(3) B11 0.038(3) 0.037(3) 0.048(4) -0.001(3) 0.005(3) -0.001(2) B12 0.033(3) 0.035(3) 0.053(4) -0.009(3) 0.000(3) -0.002(3) C13 0.042(2) 0.046(3) 0.045(3) -0.004(2) 0.002(2) 0.010(2) C14 0.053(3) 0.067(4) 0.075(4) -0.013(4) -0.004(3) 0.022(3) C15 0.065(4) 0.074(4) 0.063(4) -0.001(3) 0.023(4) 0.007(3) C16 0.060(3) 0.052(4) 0.084(5) -0.004(3) -0.005(3) 0.014(3) N' 0.039(2) 0.052(3) 0.042(3) 0.013(2) 0.006(2) 0.012(2) C1' 0.040(3) 0.034(3) 0.038(3) 0.002(2) -0.001(2) -0.006(2) B3' 0.037(3) 0.038(3) 0.031(3) -0.005(2) 0.000(2) 0.001(2) B4' 0.034(3) 0.039(3) 0.036(3) 0.001(3) 0.001(3) -0.002(2) B5' 0.037(3) 0.045(3) 0.030(3) 0.004(3) 0.003(3) 0.006(2) B6' 0.036(3) 0.035(3) 0.032(3) -0.009(2) -0.003(3) 0.003(2) C7' 0.038(2) 0.040(3) 0.035(3) 0.003(2) 0.005(2) 0.006(2) B8' 0.036(3) 0.047(3) 0.032(3) 0.001(2) 0.004(2) 0.004(3) C9' 0.032(2) 0.038(3) 0.033(3) 0.003(2) -0.001(2) 0.001(2) B10' 0.033(3) 0.048(4) 0.039(3) -0.008(3) -0.005(2) -0.001(2) B11' 0.035(3) 0.031(3) 0.056(4) -0.007(3) -0.005(3) 0.002(2) B12' 0.034(3) 0.039(4) 0.047(3) 0.012(3) 0.002(3) -0.003(2) C13' 0.042(3) 0.049(3) 0.039(3) 0.009(2) -0.002(2) 0.011(2) C14' 0.045(3) 0.092(5) 0.064(4) 0.024(4) 0.007(3) 0.023(3) C15' 0.060(3) 0.057(4) 0.067(4) 0.026(3) 0.006(3) 0.013(3) C16' 0.070(4) 0.088(4) 0.057(3) -0.003(3) -0.019(3) 0.022(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 N C9 1.416(6) . ? N C13 1.479(6) . ? N H0 0.8899(11) . ? C1 B6 1.710(7) . ? C1 B4 1.727(8) . ? C1 B5 1.735(8) . ? C1 B3 1.749(8) . ? C1 Ru2 2.183(5) . ? C1 H1 1.1000 . ? Ru2 B3 2.163(5) . ? Ru2 B6' 2.164(6) . ? Ru2 B3' 2.165(6) . ? Ru2 B6 2.179(5) . ? Ru2 B11 2.181(5) . ? Ru2 B11' 2.185(5) . ? Ru2 C1' 2.199(5) . ? Ru2 C7' 2.202(5) . ? Ru2 C7 2.208(5) . ? B3 C7 1.729(8) . ? B3 B8 1.777(8) . ? B3 B4 1.788(8) . ? B3 H3 1.1000 . ? B4 C9 1.731(7) . ? B4 B8 1.737(9) . ? B4 B5 1.776(8) . ? B4 H4 1.1000 . ? B5 C9 1.700(7) . ? B5 B6 1.752(8) . ? B5 B10 1.765(8) . ? B5 H5 1.1000 . ? B6 B10 1.742(8) . ? B6 B11 1.776(8) . ? B6 H6 1.1000 . ? C7 B12 1.693(7) . ? C7 B8 1.706(8) . ? C7 B11 1.720(8) . ? C7 H7 1.1000 . ? B8 C9 1.738(8) . ? B8 B12 1.786(9) . ? B8 H8 1.1000 . ? C9 B12 1.737(8) . ? C9 B10 1.743(7) . ? B10 B12 1.768(8) . ? B10 B11 1.799(8) . ? B10 H10 1.1000 . ? B11 B12 1.797(8) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C13 C16 1.520(8) . ? C13 C14 1.524(8) . ? C13 C15 1.540(7) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? N' C9' 1.424(6) . ? N' C13' 1.487(6) . ? N' H0' 0.8900(11) . ? C1' B5' 1.718(7) . ? C1' B4' 1.719(7) . ? C1' B6' 1.725(7) . ? C1' B3' 1.743(7) . ? C1' H1' 1.1000 . ? B3' C7' 1.737(8) . ? B3' B8' 1.790(8) . ? B3' B4' 1.796(8) . ? B3' H3' 1.1000 . ? B4' C9' 1.720(7) . ? B4' B8' 1.733(8) . ? B4' B5' 1.773(8) . ? B4' H4' 1.1000 . ? B5' C9' 1.702(7) . ? B5' B6' 1.769(7) . ? B5' B10' 1.777(8) . ? B5' H5' 1.1000 . ? B6' B10' 1.761(7) . ? B6' B11' 1.763(9) . ? B6' H6' 1.1000 . ? C7' B8' 1.711(7) . ? C7' B12' 1.712(7) . ? C7' B11' 1.730(8) . ? C7' H7' 1.1000 . ? B8' C9' 1.717(7) . ? B8' B12' 1.783(8) . ? B8' H8' 1.1000 . ? C9' B12' 1.720(7) . ? C9' B10' 1.772(7) . ? B10' B12' 1.753(8) . ? B10' B11' 1.775(8) . ? B10' H10' 1.1000 . ? B11' B12' 1.791(8) . ? B11' H11' 1.1000 . ? B12' H12' 1.1000 . ? C13' C16' 1.519(8) . ? C13' C15' 1.537(8) . ? C13' C14' 1.548(7) . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15' H15D 0.9600 . ? C15' H15E 0.9600 . ? C15' H15F 0.9600 . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? 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 C9 N C13 127.6(4) . . ? C9 N H0 115.4(10) . . ? C13 N H0 110.4(10) . . ? B6 C1 B4 110.7(4) . . ? B6 C1 B5 61.1(3) . . ? B4 C1 B5 61.7(3) . . ? B6 C1 B3 109.5(4) . . ? B4 C1 B3 61.9(3) . . ? B5 C1 B3 111.6(4) . . ? B6 C1 Ru2 66.8(2) . . ? B4 C1 Ru2 122.5(3) . . ? B5 C1 Ru2 122.9(3) . . ? B3 C1 Ru2 65.7(2) . . ? B6 C1 H1 121.5 . . ? B4 C1 H1 117.5 . . ? B5 C1 H1 117.3 . . ? B3 C1 H1 121.2 . . ? Ru2 C1 H1 108.6 . . ? B3 Ru2 B6' 146.9(2) . . ? B3 Ru2 B3' 118.6(2) . . ? B6' Ru2 B3' 81.8(2) . . ? B3 Ru2 B6 81.2(2) . . ? B6' Ru2 B6 95.1(2) . . ? B3' Ru2 B6 146.8(2) . . ? B3 Ru2 B11 82.5(2) . . ? B6' Ru2 B11 119.3(2) . . ? B3' Ru2 B11 105.1(2) . . ? B6 Ru2 B11 48.1(2) . . ? B3 Ru2 C1 47.5(2) . . ? B6' Ru2 C1 107.8(2) . . ? B3' Ru2 C1 164.7(2) . . ? B6 Ru2 C1 46.17(19) . . ? B11 Ru2 C1 80.9(2) . . ? B3 Ru2 B11' 105.7(2) . . ? B6' Ru2 B11' 47.8(2) . . ? B3' Ru2 B11' 82.6(2) . . ? B6 Ru2 B11' 119.4(2) . . ? B11 Ru2 B11' 164.7(2) . . ? C1 Ru2 B11' 95.0(2) . . ? B3 Ru2 C1' 164.4(2) . . ? B6' Ru2 C1' 46.55(19) . . ? B3' Ru2 C1' 47.08(19) . . ? B6 Ru2 C1' 108.6(2) . . ? B11 Ru2 C1' 95.0(2) . . ? C1 Ru2 C1' 147.53(19) . . ? B11' Ru2 C1' 80.5(2) . . ? B3 Ru2 C7' 96.3(2) . . ? B6' Ru2 C7' 78.6(2) . . ? B3' Ru2 C7' 46.9(2) . . ? B6 Ru2 C7' 164.6(2) . . ? B11 Ru2 C7' 147.0(2) . . ? C1 Ru2 C7' 122.1(2) . . ? B11' Ru2 C7' 46.4(2) . . ? C1' Ru2 C7' 77.4(2) . . ? B3 Ru2 C7 46.6(2) . . ? B6' Ru2 C7 164.4(2) . . ? B3' Ru2 C7 96.3(2) . . ? B6 Ru2 C7 77.98(19) . . ? B11 Ru2 C7 46.1(2) . . ? C1 Ru2 C7 77.6(2) . . ? B11' Ru2 C7 147.5(2) . . ? C1' Ru2 C7 122.2(2) . . ? C7' Ru2 C7 111.42(18) . . ? C7 B3 C1 104.5(4) . . ? C7 B3 B8 58.2(3) . . ? C1 B3 B8 104.6(4) . . ? C7 B3 B4 103.8(4) . . ? C1 B3 B4 58.4(3) . . ? B8 B3 B4 58.3(3) . . ? C7 B3 Ru2 68.1(3) . . ? C1 B3 Ru2 66.8(2) . . ? B8 B3 Ru2 121.4(4) . . ? B4 B3 Ru2 120.4(3) . . ? C7 B3 H3 124.7 . . ? C1 B3 H3 124.8 . . ? B8 B3 H3 121.0 . . ? B4 B3 H3 121.7 . . ? Ru2 B3 H3 107.3 . . ? C1 B4 C9 104.3(4) . . ? C1 B4 B8 107.3(4) . . ? C9 B4 B8 60.2(3) . . ? C1 B4 B5 59.4(3) . . ? C9 B4 B5 58.0(3) . . ? B8 B4 B5 107.9(4) . . ? C1 B4 B3 59.7(3) . . ? C9 B4 B3 106.9(4) . . ? B8 B4 B3 60.5(3) . . ? B5 B4 B3 107.9(4) . . ? C1 B4 H4 123.3 . . ? C9 B4 H4 123.8 . . ? B8 B4 H4 121.1 . . ? B5 B4 H4 122.2 . . ? B3 B4 H4 121.5 . . ? C9 B5 C1 105.2(4) . . ? C9 B5 B6 106.1(4) . . ? C1 B5 B6 58.7(3) . . ? C9 B5 B10 60.4(3) . . ? C1 B5 B10 106.4(4) . . ? B6 B5 B10 59.4(3) . . ? C9 B5 B4 59.7(3) . . ? C1 B5 B4 58.9(3) . . ? B6 B5 B4 106.5(4) . . ? B10 B5 B4 108.6(4) . . ? C9 B5 H5 122.9 . . ? C1 B5 H5 123.6 . . ? B6 B5 H5 123.0 . . ? B10 B5 H5 121.4 . . ? B4 B5 H5 121.8 . . ? C1 B6 B10 108.6(4) . . ? C1 B6 B5 60.1(3) . . ? B10 B6 B5 60.7(3) . . ? C1 B6 B11 108.7(4) . . ? B10 B6 B11 61.5(3) . . ? B5 B6 B11 110.3(4) . . ? C1 B6 Ru2 67.0(2) . . ? B10 B6 Ru2 122.1(3) . . ? B5 B6 Ru2 122.2(3) . . ? B11 B6 Ru2 66.0(2) . . ? C1 B6 H6 122.5 . . ? B10 B6 H6 118.7 . . ? B5 B6 H6 118.4 . . ? B11 B6 H6 121.5 . . ? Ru2 B6 H6 108.3 . . ? B12 C7 B8 63.4(3) . . ? B12 C7 B11 63.6(3) . . ? B8 C7 B11 115.1(4) . . ? B12 C7 B3 114.2(4) . . ? B8 C7 B3 62.3(3) . . ? B11 C7 B3 112.2(4) . . ? B12 C7 Ru2 124.0(3) . . ? B8 C7 Ru2 122.6(4) . . ? B11 C7 Ru2 66.1(2) . . ? B3 C7 Ru2 65.3(2) . . ? B12 C7 H7 115.1 . . ? B8 C7 H7 115.9 . . ? B11 C7 H7 118.8 . . ? B3 C7 H7 120.1 . . ? Ru2 C7 H7 109.4 . . ? C7 B8 B4 107.0(4) . . ? C7 B8 C9 103.4(4) . . ? B4 B8 C9 59.7(3) . . ? C7 B8 B3 59.5(3) . . ? B4 B8 B3 61.1(3) . . ? C9 B8 B3 107.0(4) . . ? C7 B8 B12 57.9(3) . . ? B4 B8 B12 108.3(4) . . ? C9 B8 B12 59.0(3) . . ? B3 B8 B12 107.5(4) . . ? C7 B8 H8 124.3 . . ? B4 B8 H8 120.9 . . ? C9 B8 H8 123.8 . . ? B3 B8 H8 121.3 . . ? B12 B8 H8 122.2 . . ? N C9 B5 125.8(4) . . ? N C9 B4 120.8(4) . . ? B5 C9 B4 62.3(3) . . ? N C9 B12 114.8(4) . . ? B5 C9 B12 111.7(4) . . ? B4 C9 B12 110.9(4) . . ? N C9 B8 114.2(4) . . ? B5 C9 B8 111.4(4) . . ? B4 C9 B8 60.1(3) . . ? B12 C9 B8 61.9(3) . . ? N C9 B10 122.4(4) . . ? B5 C9 B10 61.7(3) . . ? B4 C9 B10 111.8(4) . . ? B12 C9 B10 61.1(3) . . ? B8 C9 B10 111.2(4) . . ? B6 B10 C9 104.7(4) . . ? B6 B10 B5 59.9(3) . . ? C9 B10 B5 58.0(3) . . ? B6 B10 B12 107.5(4) . . ? C9 B10 B12 59.3(3) . . ? B5 B10 B12 107.2(4) . . ? B6 B10 B11 60.2(3) . . ? C9 B10 B11 106.7(4) . . ? B5 B10 B11 108.7(4) . . ? B12 B10 B11 60.5(3) . . ? B6 B10 H10 122.7 . . ? C9 B10 H10 124.1 . . ? B5 B10 H10 121.9 . . ? B12 B10 H10 121.7 . . ? B11 B10 H10 121.1 . . ? C7 B11 B6 104.3(4) . . ? C7 B11 B12 57.5(3) . . ? B6 B11 B12 104.8(4) . . ? C7 B11 B10 103.6(4) . . ? B6 B11 B10 58.3(3) . . ? B12 B11 B10 58.9(3) . . ? C7 B11 Ru2 67.8(2) . . ? B6 B11 Ru2 65.9(3) . . ? B12 B11 Ru2 120.1(4) . . ? B10 B11 Ru2 119.2(4) . . ? C7 B11 H11 124.9 . . ? B6 B11 H11 124.8 . . ? B12 B11 H11 121.2 . . ? B10 B11 H11 121.8 . . ? Ru2 B11 H11 108.6 . . ? C7 B12 C9 104.0(4) . . ? C7 B12 B10 106.1(4) . . ? C9 B12 B10 59.6(3) . . ? C7 B12 B8 58.7(3) . . ? C9 B12 B8 59.1(3) . . ? B10 B12 B8 107.9(4) . . ? C7 B12 B11 59.0(3) . . ? C9 B12 B11 107.0(4) . . ? B10 B12 B11 60.6(4) . . ? B8 B12 B11 107.6(4) . . ? C7 B12 H12 124.3 . . ? C9 B12 H12 123.4 . . ? B10 B12 H12 121.6 . . ? B8 B12 H12 121.9 . . ? B11 B12 H12 121.6 . . ? N C13 C16 112.2(4) . . ? N C13 C14 104.6(4) . . ? C16 C13 C14 109.3(5) . . ? N C13 C15 111.5(5) . . ? C16 C13 C15 110.9(5) . . ? C14 C13 C15 108.1(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C9' N' C13' 126.1(4) . . ? C9' N' H0' 114.3(10) . . ? C13' N' H0' 109.1(10) . . ? B5' C1' B4' 62.1(3) . . ? B5' C1' B6' 61.8(3) . . ? B4' C1' B6' 111.8(4) . . ? B5' C1' B3' 112.3(4) . . ? B4' C1' B3' 62.5(3) . . ? B6' C1' B3' 109.6(4) . . ? B5' C1' Ru2 122.4(3) . . ? B4' C1' Ru2 122.6(3) . . ? B6' C1' Ru2 65.7(2) . . ? B3' C1' Ru2 65.4(3) . . ? B5' C1' H1' 116.9 . . ? B4' C1' H1' 116.7 . . ? B6' C1' H1' 121.3 . . ? B3' C1' H1' 120.9 . . ? Ru2 C1' H1' 109.4 . . ? C7' B3' C1' 104.5(4) . . ? C7' B3' B8' 58.0(3) . . ? C1' B3' B8' 103.7(4) . . ? C7' B3' B4' 103.5(4) . . ? C1' B3' B4' 58.1(3) . . ? B8' B3' B4' 57.8(3) . . ? C7' B3' Ru2 67.7(2) . . ? C1' B3' Ru2 67.5(3) . . ? B8' B3' Ru2 120.7(4) . . ? B4' B3' Ru2 120.6(3) . . ? C7' B3' H3' 124.8 . . ? C1' B3' H3' 124.8 . . ? B8' B3' H3' 121.8 . . ? B4' B3' H3' 121.9 . . ? Ru2 B3' H3' 107.3 . . ? C1' B4' C9' 104.3(4) . . ? C1' B4' B8' 107.2(4) . . ? C9' B4' B8' 59.6(3) . . ? C1' B4' B5' 58.9(3) . . ? C9' B4' B5' 58.3(3) . . ? B8' B4' B5' 107.3(4) . . ? C1' B4' B3' 59.4(3) . . ? C9' B4' B3' 107.0(4) . . ? B8' B4' B3' 60.9(3) . . ? B5' B4' B3' 107.3(4) . . ? C1' B4' H4' 123.5 . . ? C9' B4' H4' 123.7 . . ? B8' B4' H4' 121.3 . . ? B5' B4' H4' 122.6 . . ? B3' B4' H4' 121.5 . . ? C9' B5' C1' 105.2(4) . . ? C9' B5' B6' 106.8(4) . . ? C1' B5' B6' 59.3(3) . . ? C9' B5' B4' 59.3(3) . . ? C1' B5' B4' 59.0(3) . . ? B6' B5' B4' 107.3(4) . . ? C9' B5' B10' 61.2(3) . . ? C1' B5' B10' 107.2(4) . . ? B6' B5' B10' 59.5(3) . . ? B4' B5' B10' 109.4(4) . . ? C9' B5' H5' 122.7 . . ? C1' B5' H5' 123.5 . . ? B6' B5' H5' 122.5 . . ? B4' B5' H5' 121.6 . . ? B10' B5' H5' 120.7 . . ? C1' B6' B10' 107.6(4) . . ? C1' B6' B11' 108.6(4) . . ? B10' B6' B11' 60.5(3) . . ? C1' B6' B5' 58.9(3) . . ? B10' B6' B5' 60.5(3) . . ? B11' B6' B5' 108.9(4) . . ? C1' B6' Ru2 67.8(2) . . ? B10' B6' Ru2 121.9(4) . . ? B11' B6' Ru2 66.7(3) . . ? B5' B6' Ru2 121.7(3) . . ? C1' B6' H6' 122.7 . . ? B10' B6' H6' 119.3 . . ? B11' B6' H6' 121.9 . . ? B5' B6' H6' 119.5 . . ? Ru2 B6' H6' 107.8 . . ? B8' C7' B12' 62.8(3) . . ? B8' C7' B11' 113.9(4) . . ? B12' C7' B11' 62.7(3) . . ? B8' C7' B3' 62.6(3) . . ? B12' C7' B3' 113.7(4) . . ? B11' C7' B3' 111.9(4) . . ? B8' C7' Ru2 122.7(3) . . ? B12' C7' Ru2 123.3(3) . . ? B11' C7' Ru2 66.2(2) . . ? B3' C7' Ru2 65.4(2) . . ? B8' C7' H7' 116.2 . . ? B12' C7' H7' 116.0 . . ? B11' C7' H7' 119.5 . . ? B3' C7' H7' 120.0 . . ? Ru2 C7' H7' 109.3 . . ? C7' B8' C9' 104.1(4) . . ? C7' B8' B4' 107.3(4) . . ? C9' B8' B4' 59.8(3) . . ? C7' B8' B12' 58.6(3) . . ? C9' B8' B12' 58.8(3) . . ? B4' B8' B12' 108.3(4) . . ? C7' B8' B3' 59.4(3) . . ? C9' B8' B3' 107.3(4) . . ? B4' B8' B3' 61.3(3) . . ? B12' B8' B3' 107.8(4) . . ? C7' B8' H8' 123.8 . . ? C9' B8' H8' 123.6 . . ? B4' B8' H8' 120.9 . . ? B12' B8' H8' 122.1 . . ? B3' B8' H8' 121.2 . . ? N' C9' B5' 126.0(4) . . ? N' C9' B8' 113.5(4) . . ? B5' C9' B8' 111.4(3) . . ? N' C9' B4' 119.3(4) . . ? B5' C9' B4' 62.4(3) . . ? B8' C9' B4' 60.5(3) . . ? N' C9' B12' 115.4(4) . . ? B5' C9' B12' 111.0(4) . . ? B8' C9' B12' 62.5(3) . . ? B4' C9' B12' 111.8(4) . . ? N' C9' B10' 123.4(4) . . ? B5' C9' B10' 61.5(3) . . ? B8' C9' B10' 111.2(4) . . ? B4' C9' B10' 112.1(4) . . ? B12' C9' B10' 60.2(3) . . ? B12' B10' B6' 107.4(4) . . ? B12' B10' C9' 58.4(3) . . ? B6' B10' C9' 104.1(4) . . ? B12' B10' B11' 61.0(3) . . ? B6' B10' B11' 59.8(3) . . ? C9' B10' B11' 106.0(4) . . ? B12' B10' B5' 106.0(4) . . ? B6' B10' B5' 60.0(3) . . ? C9' B10' B5' 57.3(3) . . ? B11' B10' B5' 107.9(4) . . ? B12' B10' H10' 122.1 . . ? B6' B10' H10' 122.7 . . ? C9' B10' H10' 124.9 . . ? B11' B10' H10' 121.3 . . ? B5' B10' H10' 122.6 . . ? C7' B11' B6' 104.7(4) . . ? C7' B11' B10' 104.7(4) . . ? B6' B11' B10' 59.7(3) . . ? C7' B11' B12' 58.2(3) . . ? B6' B11' B12' 105.7(4) . . ? B10' B11' B12' 58.9(3) . . ? C7' B11' Ru2 67.3(2) . . ? B6' B11' Ru2 65.5(3) . . ? B10' B11' Ru2 120.1(4) . . ? B12' B11' Ru2 120.3(4) . . ? C7' B11' H11' 124.6 . . ? B6' B11' H11' 124.3 . . ? B10' B11' H11' 120.7 . . ? B12' B11' H11' 120.9 . . ? Ru2 B11' H11' 108.7 . . ? C7' B12' C9' 103.9(4) . . ? C7' B12' B10' 106.5(4) . . ? C9' B12' B10' 61.3(3) . . ? C7' B12' B8' 58.6(3) . . ? C9' B12' B8' 58.7(3) . . ? B10' B12' B8' 109.0(4) . . ? C7' B12' B11' 59.1(3) . . ? C9' B12' B11' 107.5(4) . . ? B10' B12' B11' 60.1(4) . . ? B8' B12' B11' 107.6(4) . . ? C7' B12' H12' 124.4 . . ? C9' B12' H12' 123.0 . . ? B10' B12' H12' 120.8 . . ? B8' B12' H12' 121.9 . . ? B11' B12' H12' 121.8 . . ? N' C13' C16' 114.1(4) . . ? N' C13' C15' 110.8(4) . . ? C16' C13' C15' 111.7(5) . . ? N' C13' C14' 103.5(4) . . ? C16' C13' C14' 108.2(5) . . ? C15' C13' C14' 107.9(5) . . ? C13' C14' H14D 109.5 . . ? C13' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C13' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? C13' C15' H15D 109.5 . . ? C13' C15' H15E 109.5 . . ? H15D C15' H15E 109.5 . . ? C13' C15' H15F 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? C13' C16' H16D 109.5 . . ? C13' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C13' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.462 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.067 #===END