# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H22 O6 Ru' _chemical_formula_weight 507.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0180 0.0090 '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' O O 0.0490 0.0320 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0550 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4141(2) _cell_length_b 8.9708(4) _cell_length_c 16.1229(7) _cell_angle_alpha 79.577(4) _cell_angle_beta 84.280(3) _cell_angle_gamma 84.316(3) _cell_volume 1045.79(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4116 _cell_measurement_theta_min 5.0260 _cell_measurement_theta_max 71.7362 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 6.406 _exptl_absorpt_correction_T_min 0.2671 _exptl_absorpt_correction_T_max 0.3757 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis RED; Oxford Diffraction, 2009) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Micro-Focus (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION SUPER NOVA' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6369 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.03 _diffrn_reflns_theta_max 65.07 _reflns_number_total 3561 _reflns_number_gt 3354 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0947P)^2^+0.4328P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3561 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1297 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Ru1 Ru 0.31623(4) 0.60258(3) 0.285665(17) 0.02358(16) Uani 1 1 d . . . O1 O 0.3744(4) 0.6994(3) 0.16513(18) 0.0243(6) Uani 1 1 d . . . O2 O 0.2670(4) 0.4327(3) 0.22854(18) 0.0259(6) Uani 1 1 d . . . O3 O 0.5786(4) 0.5187(4) 0.29810(19) 0.0301(7) Uani 1 1 d . . . O4 O 0.2358(4) 0.4967(3) 0.40261(18) 0.0285(6) Uani 1 1 d . . . O5 O 0.3677(4) 0.7806(3) 0.33792(19) 0.0294(7) Uani 1 1 d . . . O6 O 0.0578(4) 0.6798(4) 0.27124(19) 0.0296(7) Uani 1 1 d . . . C1 C 0.3185(5) 0.6238(4) 0.1127(3) 0.0224(8) Uani 1 1 d . . . C2 C 0.3285(5) 0.6757(4) 0.0228(3) 0.0218(8) Uani 1 1 d . . . C3 C 0.3872(5) 0.8198(5) -0.0118(3) 0.0259(8) Uani 1 1 d . . . H3 H 0.4151 0.8850 0.0247 0.031 Uiso 1 1 calc R . . C4 C 0.4045(5) 0.8669(4) -0.0977(3) 0.0270(9) Uani 1 1 d . . . H4 H 0.4438 0.9646 -0.1208 0.032 Uiso 1 1 calc R . . C5 C 0.3637(5) 0.7702(5) -0.1513(3) 0.0297(9) Uani 1 1 d . . . H5 H 0.3776 0.8019 -0.2109 0.036 Uiso 1 1 calc R . . C6 C 0.3035(5) 0.6291(5) -0.1179(3) 0.0271(9) Uani 1 1 d . . . H6 H 0.2751 0.5653 -0.1550 0.032 Uiso 1 1 calc R . . C7 C 0.2834(5) 0.5782(4) -0.0303(3) 0.0224(8) Uani 1 1 d . . . C8 C 0.2216(5) 0.4272(4) 0.0064(3) 0.0231(8) Uani 1 1 d . . . C9 C 0.1768(5) 0.3263(5) -0.0440(3) 0.0271(9) Uani 1 1 d . . . H9 H 0.1815 0.3568 -0.1037 0.033 Uiso 1 1 calc R . . C10 C 0.1256(6) 0.1825(5) -0.0080(3) 0.0324(10) Uani 1 1 d . . . H10 H 0.0978 0.1151 -0.0432 0.039 Uiso 1 1 calc R . . C11 C 0.1148(6) 0.1363(5) 0.0796(3) 0.0321(10) Uani 1 1 d . . . H11 H 0.0798 0.0378 0.1040 0.039 Uiso 1 1 calc R . . C12 C 0.1545(5) 0.2328(5) 0.1299(3) 0.0283(9) Uani 1 1 d . . . H12 H 0.1455 0.2015 0.1896 0.034 Uiso 1 1 calc R . . C13 C 0.2088(5) 0.3784(4) 0.0948(3) 0.0221(8) Uani 1 1 d . . . C14 C 0.2589(5) 0.4764(4) 0.1482(2) 0.0223(8) Uani 1 1 d . . . C15 C 0.8267(6) 0.3569(6) 0.3496(3) 0.0394(11) Uani 1 1 d . . . H15A H 0.8474 0.3008 0.3022 0.059 Uiso 1 1 calc R . . H15B H 0.8591 0.2893 0.4018 0.059 Uiso 1 1 calc R . . H15C H 0.9023 0.4432 0.3386 0.059 Uiso 1 1 calc R . . C16 C 0.6284(6) 0.4147(5) 0.3592(3) 0.0300(9) Uani 1 1 d . . . C17 C 0.5194(6) 0.3547(5) 0.4296(3) 0.0345(10) Uani 1 1 d . . . H17 H 0.5754 0.2766 0.4690 0.041 Uiso 1 1 calc R . . C18 C 0.3341(6) 0.3973(5) 0.4489(3) 0.0303(9) Uani 1 1 d . . . C19 C 0.2397(7) 0.3217(6) 0.5296(3) 0.0380(10) Uani 1 1 d . . . H19A H 0.1341 0.3880 0.5460 0.057 Uiso 1 1 calc R . . H19B H 0.3238 0.3027 0.5742 0.057 Uiso 1 1 calc R . . H19C H 0.1993 0.2250 0.5214 0.057 Uiso 1 1 calc R . . C20 C 0.3268(8) 1.0239(6) 0.3749(4) 0.0489(13) Uani 1 1 d . . . H20A H 0.2702 1.0244 0.4324 0.073 Uiso 1 1 calc R . . H20B H 0.2964 1.1221 0.3392 0.073 Uiso 1 1 calc R . . H20C H 0.4591 1.0065 0.3763 0.073 Uiso 1 1 calc R . . C21 C 0.2571(6) 0.8986(5) 0.3389(3) 0.0307(9) Uani 1 1 d . . . C22 C 0.0818(6) 0.9187(5) 0.3114(3) 0.0345(10) Uani 1 1 d . . . H22 H 0.0173 1.0148 0.3141 0.041 Uiso 1 1 calc R . . C23 C -0.0088(6) 0.8146(5) 0.2807(3) 0.0303(9) Uani 1 1 d . . . C24 C -0.1985(6) 0.8538(6) 0.2551(3) 0.0380(11) Uani 1 1 d . . . H24A H -0.1946 0.8931 0.1942 0.057 Uiso 1 1 calc R . . H24B H -0.2595 0.9314 0.2863 0.057 Uiso 1 1 calc R . . H24C H -0.2657 0.7625 0.2681 0.057 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 Ru1 0.0244(2) 0.0240(2) 0.0232(2) -0.00638(14) -0.00128(14) -0.00268(14) O1 0.0268(14) 0.0209(14) 0.0265(15) -0.0065(12) -0.0005(11) -0.0054(11) O2 0.0278(15) 0.0243(15) 0.0257(15) -0.0054(12) 0.0024(12) -0.0051(12) O3 0.0247(15) 0.0409(18) 0.0257(15) -0.0102(14) -0.0010(12) -0.0012(13) O4 0.0293(15) 0.0315(16) 0.0245(15) -0.0073(13) 0.0029(12) -0.0023(12) O5 0.0320(16) 0.0298(16) 0.0291(16) -0.0116(13) -0.0037(12) -0.0025(13) O6 0.0246(14) 0.0372(17) 0.0280(16) -0.0086(13) -0.0016(12) -0.0029(12) C1 0.0211(18) 0.0210(19) 0.026(2) -0.0067(16) -0.0032(15) -0.0011(15) C2 0.0185(17) 0.0187(18) 0.029(2) -0.0066(15) -0.0021(15) 0.0012(14) C3 0.0217(18) 0.024(2) 0.032(2) -0.0073(17) -0.0040(16) 0.0002(15) C4 0.027(2) 0.020(2) 0.032(2) -0.0019(16) -0.0022(16) 0.0023(16) C5 0.028(2) 0.032(2) 0.027(2) -0.0027(17) -0.0032(16) 0.0026(17) C6 0.025(2) 0.030(2) 0.029(2) -0.0123(17) -0.0052(16) 0.0017(17) C7 0.0185(18) 0.0213(19) 0.028(2) -0.0077(16) -0.0046(15) 0.0040(15) C8 0.0177(18) 0.0215(19) 0.032(2) -0.0101(16) -0.0032(15) 0.0014(15) C9 0.0266(19) 0.027(2) 0.030(2) -0.0094(17) -0.0059(16) -0.0016(16) C10 0.029(2) 0.028(2) 0.045(3) -0.0178(19) -0.0040(18) -0.0049(17) C11 0.029(2) 0.021(2) 0.047(3) -0.0098(19) -0.0017(19) -0.0045(17) C12 0.027(2) 0.024(2) 0.033(2) -0.0049(17) -0.0024(17) -0.0010(16) C13 0.0170(17) 0.0189(19) 0.032(2) -0.0078(16) -0.0020(14) -0.0008(14) C14 0.0184(17) 0.0206(19) 0.026(2) -0.0035(15) 0.0018(14) 0.0019(14) C15 0.030(2) 0.038(3) 0.051(3) -0.010(2) -0.008(2) 0.0028(19) C16 0.030(2) 0.028(2) 0.036(2) -0.0133(19) -0.0089(18) -0.0009(17) C17 0.039(2) 0.028(2) 0.036(2) -0.0005(18) -0.0079(19) -0.0017(18) C18 0.041(2) 0.027(2) 0.026(2) -0.0082(17) -0.0058(18) -0.0095(18) C19 0.048(3) 0.040(3) 0.026(2) -0.0041(19) -0.0006(19) -0.013(2) C20 0.058(3) 0.038(3) 0.057(3) -0.023(2) -0.001(3) -0.012(2) C21 0.040(2) 0.026(2) 0.026(2) -0.0081(17) 0.0028(17) -0.0055(18) C22 0.041(2) 0.024(2) 0.038(2) -0.0077(18) 0.0014(19) -0.0001(18) C23 0.033(2) 0.029(2) 0.024(2) 0.0028(17) 0.0044(17) 0.0003(17) C24 0.033(2) 0.037(3) 0.039(3) 0.004(2) -0.0037(19) 0.0031(19) _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 O6 1.993(3) . ? Ru1 O2 1.997(3) . ? Ru1 O1 2.003(3) . ? Ru1 O4 2.013(3) . ? Ru1 O5 2.019(3) . ? Ru1 O3 2.031(3) . ? O1 C1 1.296(5) . ? O2 C14 1.289(5) . ? O3 C16 1.283(5) . ? O4 C18 1.273(5) . ? O5 C21 1.275(5) . ? O6 C23 1.290(5) . ? C1 C14 1.436(5) . ? C1 C2 1.437(5) . ? C2 C3 1.405(5) . ? C2 C7 1.412(5) . ? C3 C4 1.370(6) . ? C3 H3 0.9500 . ? C4 C5 1.402(6) . ? C4 H4 0.9500 . ? C5 C6 1.382(6) . ? C5 H5 0.9500 . ? C6 C7 1.402(6) . ? C6 H6 0.9500 . ? C7 C8 1.474(6) . ? C8 C9 1.403(5) . ? C8 C13 1.410(6) . ? C9 C10 1.388(6) . ? C9 H9 0.9500 . ? C10 C11 1.394(7) . ? C10 H10 0.9500 . ? C11 C12 1.358(6) . ? C11 H11 0.9500 . ? C12 C13 1.407(5) . ? C12 H12 0.9500 . ? C13 C14 1.435(5) . ? C15 C16 1.513(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.383(6) . ? C17 C18 1.409(6) . ? C17 H17 0.9500 . ? C18 C19 1.495(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.509(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.399(6) . ? C22 C23 1.387(6) . ? C22 H22 0.9500 . ? C23 C24 1.496(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 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 O6 Ru1 O2 86.33(12) . . ? O6 Ru1 O1 87.51(12) . . ? O2 Ru1 O1 80.88(11) . . ? O6 Ru1 O4 88.36(12) . . ? O2 Ru1 O4 94.60(12) . . ? O1 Ru1 O4 174.05(10) . . ? O6 Ru1 O5 93.27(12) . . ? O2 Ru1 O5 177.27(10) . . ? O1 Ru1 O5 96.41(12) . . ? O4 Ru1 O5 88.09(12) . . ? O6 Ru1 O3 178.14(10) . . ? O2 Ru1 O3 91.83(12) . . ? O1 Ru1 O3 92.00(12) . . ? O4 Ru1 O3 91.99(12) . . ? O5 Ru1 O3 88.56(12) . . ? C1 O1 Ru1 111.7(2) . . ? C14 O2 Ru1 111.8(2) . . ? C16 O3 Ru1 123.6(3) . . ? C18 O4 Ru1 124.8(3) . . ? C21 O5 Ru1 122.9(3) . . ? C23 O6 Ru1 124.0(3) . . ? O1 C1 C14 116.3(3) . . ? O1 C1 C2 123.0(3) . . ? C14 C1 C2 120.5(3) . . ? C3 C2 C7 120.6(4) . . ? C3 C2 C1 120.3(4) . . ? C7 C2 C1 119.0(3) . . ? C4 C3 C2 120.4(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 120.4(4) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 121.2(4) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C6 C7 C2 117.7(4) . . ? C6 C7 C8 121.9(4) . . ? C2 C7 C8 120.4(4) . . ? C9 C8 C13 117.6(4) . . ? C9 C8 C7 122.3(4) . . ? C13 C8 C7 120.1(3) . . ? C10 C9 C8 121.0(4) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 120.4(4) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 119.7(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 120.9(4) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C8 120.3(4) . . ? C12 C13 C14 120.4(4) . . ? C8 C13 C14 119.2(3) . . ? O2 C14 C13 122.1(3) . . ? O2 C14 C1 117.0(4) . . ? C13 C14 C1 120.7(3) . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O3 C16 C17 126.3(4) . . ? O3 C16 C15 114.1(4) . . ? C17 C16 C15 119.6(4) . . ? C16 C17 C18 126.8(4) . . ? C16 C17 H17 116.6 . . ? C18 C17 H17 116.6 . . ? O4 C18 C17 125.4(4) . . ? O4 C18 C19 115.5(4) . . ? C17 C18 C19 119.1(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 C22 126.0(4) . . ? O5 C21 C20 114.8(4) . . ? C22 C21 C20 119.2(4) . . ? C23 C22 C21 127.6(4) . . ? C23 C22 H22 116.2 . . ? C21 C22 H22 116.2 . . ? O6 C23 C22 125.0(4) . . ? O6 C23 C24 114.1(4) . . ? C22 C23 C24 120.8(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Ru1 O1 C1 -73.7(3) . . . . ? O2 Ru1 O1 C1 12.9(2) . . . . ? O4 Ru1 O1 C1 -27.7(10) . . . . ? O5 Ru1 O1 C1 -166.7(2) . . . . ? O3 Ru1 O1 C1 104.5(3) . . . . ? O6 Ru1 O2 C14 75.0(3) . . . . ? O1 Ru1 O2 C14 -13.1(2) . . . . ? O4 Ru1 O2 C14 163.0(3) . . . . ? O5 Ru1 O2 C14 -7(2) . . . . ? O3 Ru1 O2 C14 -104.8(3) . . . . ? O6 Ru1 O3 C16 -90(3) . . . . ? O2 Ru1 O3 C16 -84.2(3) . . . . ? O1 Ru1 O3 C16 -165.1(3) . . . . ? O4 Ru1 O3 C16 10.5(3) . . . . ? O5 Ru1 O3 C16 98.6(3) . . . . ? O6 Ru1 O4 C18 168.1(3) . . . . ? O2 Ru1 O4 C18 81.9(3) . . . . ? O1 Ru1 O4 C18 122.1(9) . . . . ? O5 Ru1 O4 C18 -98.6(3) . . . . ? O3 Ru1 O4 C18 -10.1(3) . . . . ? O6 Ru1 O5 C21 -10.2(3) . . . . ? O2 Ru1 O5 C21 71(2) . . . . ? O1 Ru1 O5 C21 77.7(3) . . . . ? O4 Ru1 O5 C21 -98.4(3) . . . . ? O3 Ru1 O5 C21 169.5(3) . . . . ? O2 Ru1 O6 C23 -166.0(3) . . . . ? O1 Ru1 O6 C23 -85.0(3) . . . . ? O4 Ru1 O6 C23 99.3(3) . . . . ? O5 Ru1 O6 C23 11.3(3) . . . . ? O3 Ru1 O6 C23 -160(3) . . . . ? Ru1 O1 C1 C14 -10.8(4) . . . . ? Ru1 O1 C1 C2 174.3(3) . . . . ? O1 C1 C2 C3 -5.2(6) . . . . ? C14 C1 C2 C3 -179.9(3) . . . . ? O1 C1 C2 C7 173.0(3) . . . . ? C14 C1 C2 C7 -1.6(5) . . . . ? C7 C2 C3 C4 -1.1(6) . . . . ? C1 C2 C3 C4 177.1(4) . . . . ? C2 C3 C4 C5 -0.2(6) . . . . ? C3 C4 C5 C6 1.1(6) . . . . ? C4 C5 C6 C7 -0.7(6) . . . . ? C5 C6 C7 C2 -0.6(6) . . . . ? C5 C6 C7 C8 -179.2(4) . . . . ? C3 C2 C7 C6 1.4(5) . . . . ? C1 C2 C7 C6 -176.8(3) . . . . ? C3 C2 C7 C8 -179.9(3) . . . . ? C1 C2 C7 C8 1.9(5) . . . . ? C6 C7 C8 C9 -0.9(6) . . . . ? C2 C7 C8 C9 -179.5(3) . . . . ? C6 C7 C8 C13 177.9(3) . . . . ? C2 C7 C8 C13 -0.7(5) . . . . ? C13 C8 C9 C10 -1.4(6) . . . . ? C7 C8 C9 C10 177.5(4) . . . . ? C8 C9 C10 C11 1.1(6) . . . . ? C9 C10 C11 C12 0.0(6) . . . . ? C10 C11 C12 C13 -0.8(6) . . . . ? C11 C12 C13 C8 0.5(6) . . . . ? C11 C12 C13 C14 -177.0(4) . . . . ? C9 C8 C13 C12 0.6(5) . . . . ? C7 C8 C13 C12 -178.3(3) . . . . ? C9 C8 C13 C14 178.1(3) . . . . ? C7 C8 C13 C14 -0.8(5) . . . . ? Ru1 O2 C14 C13 -174.3(3) . . . . ? Ru1 O2 C14 C1 11.3(4) . . . . ? C12 C13 C14 O2 4.3(5) . . . . ? C8 C13 C14 O2 -173.2(3) . . . . ? C12 C13 C14 C1 178.5(3) . . . . ? C8 C13 C14 C1 1.0(5) . . . . ? O1 C1 C14 O2 -0.3(5) . . . . ? C2 C1 C14 O2 174.7(3) . . . . ? O1 C1 C14 C13 -174.8(3) . . . . ? C2 C1 C14 C13 0.2(5) . . . . ? Ru1 O3 C16 C17 -7.1(6) . . . . ? Ru1 O3 C16 C15 173.0(3) . . . . ? O3 C16 C17 C18 -1.2(8) . . . . ? C15 C16 C17 C18 178.8(4) . . . . ? Ru1 O4 C18 C17 6.0(6) . . . . ? Ru1 O4 C18 C19 -173.7(3) . . . . ? C16 C17 C18 O4 1.8(7) . . . . ? C16 C17 C18 C19 -178.5(4) . . . . ? Ru1 O5 C21 C22 5.5(6) . . . . ? Ru1 O5 C21 C20 -175.5(3) . . . . ? O5 C21 C22 C23 2.4(8) . . . . ? C20 C21 C22 C23 -176.5(4) . . . . ? Ru1 O6 C23 C22 -7.8(6) . . . . ? Ru1 O6 C23 C24 172.0(3) . . . . ? C21 C22 C23 O6 -1.2(7) . . . . ? C21 C22 C23 C24 179.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 65.07 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.978 _refine_diff_density_min -1.002 _refine_diff_density_rms 0.143 _database_code_depnum_ccdc_archive 'CCDC 963958' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H112 N7 O14 Ru3.50' _chemical_formula_weight 1941.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.1917(4) _cell_length_b 20.7180(4) _cell_length_c 36.2929(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.970(2) _cell_angle_gamma 90.00 _cell_volume 18211.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23201 _cell_measurement_theta_min 3.0173 _cell_measurement_theta_max 32.6403 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8024 _exptl_absorpt_coefficient_mu 0.637 _exptl_absorpt_correction_T_min 0.8173 _exptl_absorpt_correction_T_max 0.8778 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Micro-Focus (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION SUPER NOVA' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70181 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_unetI/netI 0.0347 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16028 _reflns_number_gt 13500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0424P)^2^+18.1572P] 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 RIDING _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16028 _refine_ls_number_parameters 1048 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.268668(9) 0.420899(11) 0.434485(6) 0.02380(6) Uani 1 1 d . . . Ru2 Ru 0.393697(9) 0.365097(10) 0.349896(6) 0.02177(6) Uani 1 1 d . . . Ru3 Ru 0.412496(10) 0.008808(12) 0.527646(6) 0.02808(7) Uani 1 1 d . . . Ru4 Ru 0.5000 0.367995(15) 0.2500 0.02381(8) Uani 1 2 d S . . O1 O 0.29525(9) 0.47233(9) 0.48328(6) 0.0314(5) Uani 1 1 d . . . O2 O 0.32994(8) 0.35360(9) 0.45330(6) 0.0303(5) Uani 1 1 d . . . O3 O 0.22175(8) 0.36777(9) 0.46271(5) 0.0298(5) Uani 1 1 d . . . O4 O 0.24156(8) 0.36344(9) 0.38683(5) 0.0278(4) Uani 1 1 d . . . O5 O 0.42009(8) 0.42008(9) 0.39862(5) 0.0253(4) Uani 1 1 d . . . O6 O 0.47236(8) 0.32681(9) 0.35887(5) 0.0268(4) Uani 1 1 d . . . O7 O 0.37737(8) 0.29309(9) 0.38443(5) 0.0274(4) Uani 1 1 d . . . O8 O 0.37237(8) 0.30734(9) 0.30413(5) 0.0294(4) Uani 1 1 d . . . O9 O 0.46373(8) 0.08653(10) 0.52963(6) 0.0339(5) Uani 1 1 d . . . O10 O 0.40402(8) 0.03272(10) 0.58138(5) 0.0319(5) Uani 1 1 d . . . O11 O 0.48375(8) -0.04146(10) 0.55323(5) 0.0317(5) Uani 1 1 d . . . O12 O 0.36516(8) -0.06829(10) 0.53099(6) 0.0350(5) Uani 1 1 d . . . O13 O 0.41618(8) 0.37029(9) 0.23416(6) 0.0305(5) Uani 1 1 d . . . O14 O 0.49938(8) 0.44038(9) 0.20988(5) 0.0281(4) Uani 1 1 d . . . N1 N 0.21530(10) 0.49018(11) 0.41273(6) 0.0268(5) Uani 1 1 d . . . H1N H 0.1816 0.4897 0.4154 0.032 Uiso 1 1 calc R . . N2 N 0.31114(9) 0.47517(11) 0.40882(6) 0.0244(5) Uani 1 1 d . . . H2N H 0.3447 0.4642 0.4084 0.029 Uiso 1 1 calc R . . N3 N 0.31936(9) 0.40273(11) 0.33699(6) 0.0242(5) Uani 1 1 d . . . H3N H 0.2946 0.3895 0.3483 0.029 Uiso 1 1 calc R . . N4 N 0.39981(9) 0.43454(11) 0.31446(6) 0.0237(5) Uani 1 1 d . . . H4N H 0.4316 0.4438 0.3101 0.028 Uiso 1 1 calc R . . N5 N 0.34447(10) 0.05039(12) 0.49655(7) 0.0304(6) Uani 1 1 d . . . H5N H 0.3246 0.0758 0.5070 0.036 Uiso 1 1 calc R . . N6 N 0.41414(10) -0.01328(12) 0.47569(7) 0.0313(6) Uani 1 1 d . . . H6N H 0.4429 -0.0329 0.4714 0.038 Uiso 1 1 calc R . . N7 N 0.50657(9) 0.29448(11) 0.21753(6) 0.0262(5) Uani 1 1 d . . . H7N H 0.5097 0.3004 0.1942 0.031 Uiso 1 1 calc R . . C1 C 0.23202(11) 0.53705(13) 0.39419(7) 0.0242(6) Uani 1 1 d . . . C2 C 0.19928(12) 0.59090(13) 0.37476(8) 0.0267(6) Uani 1 1 d . . . C3 C 0.14326(12) 0.59719(15) 0.37376(8) 0.0329(7) Uani 1 1 d . . . H3 H 0.1271 0.5669 0.3871 0.039 Uiso 1 1 calc R . . C4 C 0.11181(14) 0.64637(16) 0.35386(9) 0.0406(8) Uani 1 1 d . . . H4 H 0.0739 0.6497 0.3530 0.049 Uiso 1 1 calc R . . C5 C 0.13565(15) 0.69164(17) 0.33480(9) 0.0444(8) Uani 1 1 d . . . H5 H 0.1139 0.7261 0.3212 0.053 Uiso 1 1 calc R . . C6 C 0.19021(14) 0.68673(16) 0.33562(9) 0.0385(8) Uani 1 1 d . . . H6 H 0.2058 0.7181 0.3226 0.046 Uiso 1 1 calc R . . C7 C 0.22367(13) 0.63629(14) 0.35531(8) 0.0289(6) Uani 1 1 d . . . C8 C 0.28173(13) 0.62992(14) 0.35512(8) 0.0292(7) Uani 1 1 d . . . C9 C 0.30752(15) 0.67544(16) 0.33719(10) 0.0430(8) Uani 1 1 d . . . H9 H 0.2873 0.7124 0.3257 0.052 Uiso 1 1 calc R . . C10 C 0.36104(16) 0.66812(18) 0.33585(11) 0.0511(9) Uani 1 1 d . . . H10 H 0.3772 0.6995 0.3232 0.061 Uiso 1 1 calc R . . C11 C 0.39166(14) 0.61506(16) 0.35285(10) 0.0427(8) Uani 1 1 d . . . H11 H 0.4289 0.6103 0.3522 0.051 Uiso 1 1 calc R . . C12 C 0.36778(13) 0.56933(15) 0.37075(8) 0.0335(7) Uani 1 1 d . . . H12 H 0.3886 0.5327 0.3821 0.040 Uiso 1 1 calc R . . C13 C 0.31334(12) 0.57604(13) 0.37249(8) 0.0261(6) Uani 1 1 d . . . C14 C 0.28799(11) 0.52874(13) 0.39205(7) 0.0239(6) Uani 1 1 d . . . C15 C 0.35578(16) 0.51395(17) 0.53898(10) 0.0485(9) Uani 1 1 d . . . H15A H 0.3544 0.5573 0.5280 0.073 Uiso 1 1 calc R . . H15B H 0.3929 0.5058 0.5558 0.073 Uiso 1 1 calc R . . H15C H 0.3287 0.5107 0.5538 0.073 Uiso 1 1 calc R . . C16 C 0.34246(13) 0.46461(15) 0.50711(9) 0.0342(7) Uani 1 1 d . . . C17 C 0.38065(13) 0.41649(16) 0.50586(9) 0.0377(7) Uani 1 1 d . . . H17 H 0.4155 0.4191 0.5245 0.045 Uiso 1 1 calc R . . C18 C 0.37321(12) 0.36469(15) 0.48012(9) 0.0326(7) Uani 1 1 d . . . C19 C 0.41923(13) 0.31669(17) 0.48360(10) 0.0431(8) Uani 1 1 d . . . H19A H 0.4061 0.2734 0.4876 0.065 Uiso 1 1 calc R . . H19B H 0.4504 0.3283 0.5054 0.065 Uiso 1 1 calc R . . H19C H 0.4311 0.3171 0.4600 0.065 Uiso 1 1 calc R . . C20 C 0.16647(16) 0.28473(17) 0.47619(10) 0.0497(9) Uani 1 1 d . . . H20A H 0.1946 0.2713 0.4994 0.075 Uiso 1 1 calc R . . H20B H 0.1463 0.2467 0.4636 0.075 Uiso 1 1 calc R . . H20C H 0.1406 0.3146 0.4831 0.075 Uiso 1 1 calc R . . C21 C 0.19389(13) 0.31779(14) 0.44930(9) 0.0347(7) Uani 1 1 d . . . C22 C 0.18671(14) 0.29292(15) 0.41289(9) 0.0404(8) Uani 1 1 d . . . H22 H 0.1637 0.2559 0.4067 0.049 Uiso 1 1 calc R . . C23 C 0.20909(12) 0.31550(14) 0.38424(9) 0.0316(7) Uani 1 1 d . . . C24 C 0.19395(15) 0.28217(17) 0.34604(9) 0.0456(8) Uani 1 1 d . . . H24A H 0.1624 0.3042 0.3287 0.068 Uiso 1 1 calc R . . H24B H 0.1841 0.2372 0.3493 0.068 Uiso 1 1 calc R . . H24C H 0.2255 0.2833 0.3351 0.068 Uiso 1 1 calc R . . C25 C 0.30791(11) 0.44870(13) 0.31062(7) 0.0241(6) Uani 1 1 d . . . C26 C 0.25500(12) 0.48036(14) 0.29550(8) 0.0276(6) Uani 1 1 d . . . C27 C 0.20822(12) 0.46356(16) 0.30744(8) 0.0340(7) Uani 1 1 d . . . H27 H 0.2110 0.4305 0.3260 0.041 Uiso 1 1 calc R . . C28 C 0.15894(13) 0.49410(17) 0.29266(9) 0.0413(8) Uani 1 1 d . . . H28 H 0.1279 0.4829 0.3014 0.050 Uiso 1 1 calc R . . C29 C 0.15402(14) 0.54144(18) 0.26492(10) 0.0459(9) Uani 1 1 d . . . H29 H 0.1195 0.5621 0.2543 0.055 Uiso 1 1 calc R . . C30 C 0.19916(14) 0.55829(16) 0.25288(9) 0.0406(8) Uani 1 1 d . . . H30 H 0.1951 0.5903 0.2336 0.049 Uiso 1 1 calc R . . C31 C 0.25093(12) 0.52992(14) 0.26805(8) 0.0300(7) Uani 1 1 d . . . C32 C 0.29995(13) 0.55128(14) 0.25678(8) 0.0306(7) Uani 1 1 d . . . C33 C 0.29871(15) 0.60605(16) 0.23350(9) 0.0407(8) Uani 1 1 d . . . H33 H 0.2650 0.6291 0.2243 0.049 Uiso 1 1 calc R . . C34 C 0.34443(16) 0.62704(16) 0.22368(9) 0.0447(9) Uani 1 1 d . . . H34 H 0.3424 0.6648 0.2085 0.054 Uiso 1 1 calc R . . C35 C 0.39361(15) 0.59345(15) 0.23581(9) 0.0402(8) Uani 1 1 d . . . H35 H 0.4251 0.6071 0.2282 0.048 Uiso 1 1 calc R . . C36 C 0.39672(13) 0.54014(14) 0.25891(8) 0.0328(7) Uani 1 1 d . . . H36 H 0.4305 0.5172 0.2673 0.039 Uiso 1 1 calc R . . C37 C 0.35075(12) 0.51936(13) 0.27012(8) 0.0277(6) Uani 1 1 d . . . C38 C 0.35480(11) 0.46662(13) 0.29758(8) 0.0240(6) Uani 1 1 d . . . C39 C 0.47918(13) 0.46846(16) 0.45290(9) 0.0373(7) Uani 1 1 d . . . H39A H 0.4802 0.5122 0.4428 0.056 Uiso 1 1 calc R . . H39B H 0.5145 0.4590 0.4717 0.056 Uiso 1 1 calc R . . H39C H 0.4492 0.4653 0.4653 0.056 Uiso 1 1 calc R . . C40 C 0.46946(12) 0.42067(14) 0.42056(8) 0.0279(6) Uani 1 1 d . . . C41 C 0.51329(12) 0.38307(14) 0.41667(8) 0.0306(7) Uani 1 1 d . . . H41 H 0.5471 0.3875 0.4362 0.037 Uiso 1 1 calc R . . C42 C 0.51332(12) 0.33953(14) 0.38733(8) 0.0282(6) Uani 1 1 d . . . C43 C 0.56604(13) 0.30469(17) 0.38800(10) 0.0430(8) Uani 1 1 d . . . H43A H 0.5599 0.2580 0.3881 0.065 Uiso 1 1 calc R . . H43B H 0.5949 0.3169 0.4111 0.065 Uiso 1 1 calc R . . H43C H 0.5776 0.3165 0.3652 0.065 Uiso 1 1 calc R . . C44 C 0.32564(14) 0.20823(15) 0.40035(9) 0.0389(8) Uani 1 1 d . . . H44A H 0.3575 0.1885 0.4186 0.058 Uiso 1 1 calc R . . H44B H 0.3002 0.1744 0.3873 0.058 Uiso 1 1 calc R . . H44C H 0.3066 0.2369 0.4140 0.058 Uiso 1 1 calc R . . C45 C 0.34502(12) 0.24670(14) 0.37115(9) 0.0309(7) Uani 1 1 d . . . C46 C 0.32686(14) 0.22860(15) 0.33225(9) 0.0387(8) Uani 1 1 d . . . H46 H 0.3013 0.1939 0.3260 0.046 Uiso 1 1 calc R . . C47 C 0.34288(14) 0.25673(15) 0.30234(9) 0.0357(7) Uani 1 1 d . . . C48 C 0.32610(19) 0.22770(18) 0.26252(10) 0.0608(12) Uani 1 1 d . . . H48A H 0.3285 0.2607 0.2437 0.091 Uiso 1 1 calc R . . H48B H 0.2881 0.2118 0.2569 0.091 Uiso 1 1 calc R . . H48C H 0.3508 0.1918 0.2612 0.091 Uiso 1 1 calc R . . C49 C 0.33005(12) 0.03841(14) 0.45944(8) 0.0286(6) Uani 1 1 d . . . C50 C 0.27928(12) 0.05846(14) 0.43169(8) 0.0289(6) Uani 1 1 d . . . C51 C 0.23939(13) 0.09537(15) 0.44250(9) 0.0347(7) Uani 1 1 d . . . H51 H 0.2458 0.1081 0.4685 0.042 Uiso 1 1 calc R . . C52 C 0.19121(13) 0.11341(16) 0.41617(9) 0.0383(8) Uani 1 1 d . . . H52 H 0.1645 0.1385 0.4239 0.046 Uiso 1 1 calc R . . C53 C 0.18190(14) 0.09466(17) 0.37823(10) 0.0424(8) Uani 1 1 d . . . H53 H 0.1484 0.1065 0.3600 0.051 Uiso 1 1 calc R . . C54 C 0.22044(13) 0.05927(16) 0.36671(9) 0.0389(8) Uani 1 1 d . . . H54 H 0.2131 0.0470 0.3406 0.047 Uiso 1 1 calc R . . C55 C 0.27021(12) 0.04081(14) 0.39257(8) 0.0316(7) Uani 1 1 d . . . C56 C 0.31297(13) 0.00488(14) 0.38027(8) 0.0322(7) Uani 1 1 d . . . C57 C 0.30584(14) -0.01159(16) 0.34136(9) 0.0404(8) Uani 1 1 d . . . H57 H 0.2729 0.0009 0.3228 0.049 Uiso 1 1 calc R . . C58 C 0.34542(15) -0.04512(17) 0.32985(9) 0.0457(9) Uani 1 1 d . . . H58 H 0.3396 -0.0558 0.3036 0.055 Uiso 1 1 calc R . . C59 C 0.39387(14) -0.06335(16) 0.35645(9) 0.0402(8) Uani 1 1 d . . . H59 H 0.4209 -0.0873 0.3485 0.048 Uiso 1 1 calc R . . C60 C 0.40279(13) -0.04673(15) 0.39434(9) 0.0359(7) Uani 1 1 d . . . H60 H 0.4367 -0.0580 0.4123 0.043 Uiso 1 1 calc R . . C61 C 0.36271(12) -0.01345(14) 0.40690(8) 0.0296(7) Uani 1 1 d . . . C62 C 0.37075(12) 0.00209(14) 0.44720(8) 0.0280(6) Uani 1 1 d . . . C63 C 0.51264(15) 0.18195(17) 0.55033(11) 0.0491(9) Uani 1 1 d . . . H63A H 0.5480 0.1637 0.5492 0.074 Uiso 1 1 calc R . . H63B H 0.5188 0.2127 0.5716 0.074 Uiso 1 1 calc R . . H63C H 0.4953 0.2043 0.5262 0.074 Uiso 1 1 calc R . . C64 C 0.47537(13) 0.12867(15) 0.55631(9) 0.0346(7) Uani 1 1 d . . . C65 C 0.45793(14) 0.12788(16) 0.58947(9) 0.0400(8) Uani 1 1 d . . . H65 H 0.4698 0.1629 0.6066 0.048 Uiso 1 1 calc R . . C66 C 0.42506(12) 0.08177(16) 0.60046(8) 0.0330(7) Uani 1 1 d . . . C67 C 0.41370(15) 0.08696(18) 0.63924(9) 0.0463(9) Uani 1 1 d . . . H67A H 0.3739 0.0833 0.6360 0.069 Uiso 1 1 calc R . . H67B H 0.4269 0.1288 0.6508 0.069 Uiso 1 1 calc R . . H67C H 0.4330 0.0521 0.6559 0.069 Uiso 1 1 calc R . . C68 C 0.54201(14) -0.13193(17) 0.56197(9) 0.0423(8) Uani 1 1 d . . . H68A H 0.5544 -0.1333 0.5386 0.063 Uiso 1 1 calc R . . H68B H 0.5409 -0.1759 0.5717 0.063 Uiso 1 1 calc R . . H68C H 0.5677 -0.1057 0.5814 0.063 Uiso 1 1 calc R . . C69 C 0.48532(13) -0.10272(16) 0.55299(8) 0.0345(7) Uani 1 1 d . . . C70 C 0.43948(14) -0.14374(16) 0.54553(9) 0.0395(8) Uani 1 1 d . . . H70 H 0.4469 -0.1888 0.5461 0.047 Uiso 1 1 calc R . . C71 C 0.38414(14) -0.12574(16) 0.53736(8) 0.0368(8) Uani 1 1 d . . . C72 C 0.34072(15) -0.17594(17) 0.53660(10) 0.0476(9) Uani 1 1 d . . . H72A H 0.3312 -0.1754 0.5610 0.071 Uiso 1 1 calc R . . H72B H 0.3549 -0.2186 0.5326 0.071 Uiso 1 1 calc R . . H72C H 0.3077 -0.1665 0.5156 0.071 Uiso 1 1 calc R . . C73 C 0.50616(11) 0.23630(13) 0.23161(8) 0.0249(6) Uani 1 1 d . . . C74 C 0.51598(11) 0.17574(14) 0.21439(8) 0.0270(6) Uani 1 1 d . . . C75 C 0.53347(13) 0.17451(15) 0.18073(9) 0.0342(7) Uani 1 1 d . . . H75 H 0.5409 0.2139 0.1697 0.041 Uiso 1 1 calc R . . C76 C 0.53982(14) 0.11685(17) 0.16373(9) 0.0419(8) Uani 1 1 d . . . H76 H 0.5528 0.1165 0.1415 0.050 Uiso 1 1 calc R . . C77 C 0.52735(14) 0.05937(16) 0.17885(10) 0.0435(8) Uani 1 1 d . . . H77 H 0.5297 0.0198 0.1662 0.052 Uiso 1 1 calc R . . C78 C 0.51160(13) 0.05951(15) 0.21228(9) 0.0372(7) Uani 1 1 d . . . H78 H 0.5036 0.0196 0.2225 0.045 Uiso 1 1 calc R . . C79 C 0.50711(11) 0.11691(14) 0.23156(8) 0.0278(6) Uani 1 1 d . . . C80 C 0.32453(13) 0.38711(18) 0.19901(10) 0.0461(9) Uani 1 1 d . . . H80A H 0.3148 0.3436 0.1888 0.069 Uiso 1 1 calc R . . H80B H 0.3035 0.4189 0.1808 0.069 Uiso 1 1 calc R . . H80C H 0.3157 0.3916 0.2235 0.069 Uiso 1 1 calc R . . C81 C 0.38544(12) 0.39828(14) 0.20494(9) 0.0321(7) Uani 1 1 d . . . C82 C 0.40349(13) 0.43753(15) 0.17957(9) 0.0351(7) Uani 1 1 d . . . H82 H 0.3762 0.4518 0.1574 0.042 Uiso 1 1 calc R . . C83 C 0.45705(13) 0.45774(14) 0.18344(8) 0.0300(7) Uani 1 1 d . . . C84 C 0.46832(15) 0.50586(16) 0.15533(9) 0.0432(8) Uani 1 1 d . . . H84A H 0.4827 0.5459 0.1688 0.065 Uiso 1 1 calc R . . H84B H 0.4340 0.5150 0.1355 0.065 Uiso 1 1 calc R . . H84C H 0.4956 0.4880 0.1434 0.065 Uiso 1 1 calc R . . C101 C 0.2819(2) 0.8335(2) 0.41984(15) 0.0821(14) Uani 1 1 d . . . H10A H 0.3083 0.8611 0.4385 0.098 Uiso 1 1 calc R . . H10B H 0.2928 0.8339 0.3956 0.098 Uiso 1 1 calc R . . C102 C 0.2255(2) 0.8618(3) 0.41252(16) 0.0927(17) Uani 1 1 d . . . H10C H 0.1989 0.8343 0.3945 0.139 Uiso 1 1 calc R . . H10D H 0.2252 0.9050 0.4015 0.139 Uiso 1 1 calc R . . H10E H 0.2155 0.8647 0.4367 0.139 Uiso 1 1 calc R . . C110 C 0.28647(18) 0.7644(2) 0.43525(12) 0.0612(11) Uani 1 1 d . . . H11A H 0.2736 0.7639 0.4587 0.073 Uiso 1 1 calc R . . H11B H 0.2611 0.7367 0.4160 0.073 Uiso 1 1 calc R . . C777 C 0.4047(3) 0.6405(3) 0.47025(15) 0.105(2) Uani 1 1 d . . . H77A H 0.4165 0.6415 0.4467 0.157 Uiso 1 1 calc R . . H77B H 0.4040 0.5957 0.4788 0.157 Uiso 1 1 calc R . . H77C H 0.4307 0.6655 0.4902 0.157 Uiso 1 1 calc R . . C888 C 0.3482(2) 0.6692(2) 0.46270(13) 0.0749(13) Uani 1 1 d . . . H88A H 0.3383 0.6721 0.4872 0.090 Uiso 1 1 calc R . . H88B H 0.3214 0.6398 0.4456 0.090 Uiso 1 1 calc R . . C999 C 0.34280(18) 0.7352(2) 0.44464(11) 0.0635(11) Uani 1 1 d . . . H99A H 0.3688 0.7647 0.4623 0.076 Uiso 1 1 calc R . . H99B H 0.3544 0.7324 0.4207 0.076 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 Ru1 0.02337(12) 0.02711(13) 0.02376(12) 0.00075(9) 0.01127(10) 0.00209(9) Ru2 0.02220(12) 0.02492(12) 0.02047(12) 0.00038(9) 0.00972(10) 0.00136(9) Ru3 0.02401(13) 0.03967(14) 0.02280(13) 0.00092(10) 0.01021(10) 0.00218(10) Ru4 0.02180(17) 0.02972(18) 0.02272(17) 0.000 0.01085(14) 0.000 O1 0.0351(12) 0.0338(11) 0.0286(11) -0.0032(9) 0.0141(10) 0.0010(9) O2 0.0296(11) 0.0324(11) 0.0314(11) 0.0059(9) 0.0128(10) 0.0057(9) O3 0.0314(11) 0.0333(11) 0.0292(11) 0.0027(9) 0.0160(9) 0.0011(9) O4 0.0273(11) 0.0321(11) 0.0262(10) -0.0003(8) 0.0111(9) 0.0014(9) O5 0.0245(11) 0.0302(11) 0.0223(10) -0.0018(8) 0.0083(9) 0.0022(8) O6 0.0274(11) 0.0299(11) 0.0265(11) 0.0007(8) 0.0131(9) 0.0036(9) O7 0.0287(11) 0.0307(11) 0.0257(10) 0.0022(8) 0.0122(9) 0.0000(9) O8 0.0340(11) 0.0326(11) 0.0246(10) -0.0040(8) 0.0134(9) -0.0026(9) O9 0.0297(11) 0.0437(13) 0.0313(12) 0.0028(10) 0.0134(10) -0.0026(9) O10 0.0287(11) 0.0444(13) 0.0254(11) 0.0003(9) 0.0121(9) 0.0021(10) O11 0.0269(11) 0.0439(13) 0.0255(11) 0.0027(9) 0.0089(9) 0.0034(9) O12 0.0301(11) 0.0451(13) 0.0310(11) -0.0021(10) 0.0103(10) -0.0036(10) O13 0.0248(11) 0.0365(12) 0.0326(12) -0.0002(9) 0.0121(10) -0.0023(9) O14 0.0261(11) 0.0341(11) 0.0271(10) 0.0029(9) 0.0125(9) 0.0005(9) N1 0.0237(12) 0.0316(13) 0.0288(13) -0.0005(10) 0.0134(11) 0.0031(10) N2 0.0218(12) 0.0301(13) 0.0233(12) -0.0009(10) 0.0096(10) 0.0022(10) N3 0.0221(12) 0.0314(13) 0.0219(12) -0.0018(10) 0.0106(10) -0.0022(10) N4 0.0217(12) 0.0285(12) 0.0241(12) -0.0012(10) 0.0118(10) -0.0009(10) N5 0.0268(13) 0.0387(14) 0.0284(13) 0.0021(11) 0.0123(11) 0.0035(11) N6 0.0261(13) 0.0427(15) 0.0280(13) 0.0020(11) 0.0123(12) 0.0064(11) N7 0.0259(13) 0.0350(14) 0.0210(12) 0.0012(10) 0.0120(11) -0.0015(10) C1 0.0252(15) 0.0285(15) 0.0208(14) -0.0059(11) 0.0096(12) -0.0005(12) C2 0.0298(16) 0.0308(16) 0.0195(14) -0.0029(12) 0.0070(12) 0.0046(12) C3 0.0297(16) 0.0412(18) 0.0283(16) -0.0029(13) 0.0088(14) 0.0066(14) C4 0.0349(18) 0.052(2) 0.0338(18) 0.0014(15) 0.0070(15) 0.0159(16) C5 0.049(2) 0.047(2) 0.0336(18) 0.0073(15) 0.0052(16) 0.0202(17) C6 0.046(2) 0.0391(18) 0.0312(17) 0.0097(14) 0.0122(15) 0.0094(15) C7 0.0361(17) 0.0293(16) 0.0204(14) -0.0035(12) 0.0064(13) 0.0041(13) C8 0.0349(17) 0.0327(16) 0.0216(15) -0.0033(12) 0.0106(13) -0.0009(13) C9 0.051(2) 0.0352(18) 0.045(2) 0.0112(15) 0.0187(18) 0.0057(16) C10 0.057(2) 0.047(2) 0.059(2) 0.0140(18) 0.031(2) -0.0037(18) C11 0.041(2) 0.0434(19) 0.051(2) -0.0007(16) 0.0266(18) -0.0039(16) C12 0.0365(18) 0.0337(17) 0.0343(17) -0.0014(13) 0.0162(15) -0.0006(14) C13 0.0279(15) 0.0295(15) 0.0224(14) -0.0031(12) 0.0092(13) 0.0001(12) C14 0.0243(15) 0.0293(15) 0.0189(14) -0.0044(11) 0.0074(12) 0.0016(12) C15 0.055(2) 0.052(2) 0.040(2) -0.0098(16) 0.0143(18) -0.0173(18) C16 0.0379(19) 0.0370(17) 0.0308(17) -0.0003(13) 0.0145(15) -0.0118(14) C17 0.0270(16) 0.052(2) 0.0333(17) 0.0025(15) 0.0061(14) -0.0036(15) C18 0.0265(16) 0.0397(18) 0.0350(17) 0.0122(14) 0.0145(15) 0.0006(13) C19 0.0307(17) 0.051(2) 0.050(2) 0.0171(16) 0.0157(16) 0.0084(15) C20 0.062(2) 0.0405(19) 0.059(2) 0.0031(17) 0.037(2) -0.0090(17) C21 0.0346(17) 0.0300(17) 0.0465(19) 0.0058(14) 0.0229(16) 0.0036(14) C22 0.044(2) 0.0340(18) 0.049(2) -0.0071(15) 0.0229(17) -0.0099(15) C23 0.0283(16) 0.0322(16) 0.0358(17) -0.0040(13) 0.0111(14) 0.0025(13) C24 0.048(2) 0.046(2) 0.043(2) -0.0126(16) 0.0146(17) -0.0053(17) C25 0.0259(15) 0.0266(15) 0.0198(14) -0.0042(11) 0.0066(12) 0.0008(12) C26 0.0261(15) 0.0345(16) 0.0207(14) -0.0058(12) 0.0041(12) 0.0025(12) C27 0.0278(17) 0.0457(19) 0.0273(16) -0.0035(14) 0.0056(14) 0.0011(14) C28 0.0244(16) 0.060(2) 0.0382(19) -0.0026(16) 0.0064(15) 0.0045(15) C29 0.0312(18) 0.059(2) 0.041(2) -0.0028(17) 0.0005(16) 0.0142(16) C30 0.0383(19) 0.045(2) 0.0333(18) 0.0033(15) 0.0013(15) 0.0093(15) C31 0.0312(16) 0.0331(16) 0.0231(15) -0.0040(12) 0.0031(13) 0.0049(13) C32 0.0364(17) 0.0339(16) 0.0191(14) -0.0014(12) 0.0037(13) 0.0035(13) C33 0.048(2) 0.0413(19) 0.0291(17) 0.0073(14) 0.0042(16) 0.0123(16) C34 0.064(2) 0.0385(19) 0.0327(18) 0.0102(14) 0.0147(18) 0.0022(17) C35 0.050(2) 0.0400(19) 0.0339(18) 0.0072(14) 0.0176(16) -0.0014(16) C36 0.0385(18) 0.0330(17) 0.0297(16) 0.0025(13) 0.0140(14) 0.0017(14) C37 0.0352(17) 0.0275(15) 0.0212(14) -0.0020(12) 0.0090(13) 0.0006(13) C38 0.0243(15) 0.0245(14) 0.0241(14) -0.0058(11) 0.0083(12) -0.0017(12) C39 0.0336(18) 0.0422(19) 0.0359(18) -0.0123(14) 0.0091(15) -0.0046(14) C40 0.0293(16) 0.0311(16) 0.0251(15) 0.0023(12) 0.0107(13) -0.0026(13) C41 0.0223(15) 0.0384(17) 0.0304(16) -0.0024(13) 0.0058(13) 0.0012(13) C42 0.0270(16) 0.0306(16) 0.0290(16) 0.0075(13) 0.0114(14) 0.0030(13) C43 0.0330(18) 0.050(2) 0.046(2) 0.0012(16) 0.0103(16) 0.0136(16) C44 0.0413(19) 0.0374(18) 0.0424(19) 0.0093(14) 0.0190(16) -0.0009(15) C45 0.0293(16) 0.0302(16) 0.0383(17) 0.0067(13) 0.0177(14) 0.0063(13) C46 0.045(2) 0.0339(17) 0.0408(19) -0.0070(14) 0.0181(16) -0.0135(15) C47 0.0420(19) 0.0341(17) 0.0319(17) -0.0071(13) 0.0117(15) -0.0028(15) C48 0.096(3) 0.052(2) 0.039(2) -0.0184(17) 0.026(2) -0.031(2) C49 0.0266(15) 0.0346(16) 0.0272(16) 0.0046(12) 0.0118(13) -0.0014(13) C50 0.0284(16) 0.0310(16) 0.0296(16) 0.0061(12) 0.0118(13) -0.0020(13) C51 0.0314(17) 0.0432(18) 0.0325(17) 0.0071(14) 0.0140(15) -0.0006(14) C52 0.0334(18) 0.0410(19) 0.044(2) 0.0087(15) 0.0160(16) 0.0073(15) C53 0.0305(18) 0.052(2) 0.0402(19) 0.0122(16) 0.0024(15) 0.0049(15) C54 0.0379(19) 0.0441(19) 0.0328(17) 0.0031(14) 0.0065(15) -0.0016(15) C55 0.0293(16) 0.0330(16) 0.0317(16) 0.0067(13) 0.0071(14) -0.0044(13) C56 0.0339(17) 0.0358(17) 0.0276(16) 0.0015(13) 0.0096(14) -0.0051(14) C57 0.0387(19) 0.053(2) 0.0277(17) 0.0016(15) 0.0064(15) 0.0000(16) C58 0.055(2) 0.058(2) 0.0267(17) -0.0067(15) 0.0147(17) -0.0031(18) C59 0.045(2) 0.046(2) 0.0329(18) -0.0038(15) 0.0173(16) 0.0016(16) C60 0.0355(18) 0.0449(19) 0.0294(17) -0.0007(14) 0.0122(14) 0.0001(15) C61 0.0312(16) 0.0328(16) 0.0261(15) 0.0011(12) 0.0102(13) -0.0034(13) C62 0.0269(16) 0.0328(16) 0.0263(15) 0.0027(12) 0.0104(13) -0.0024(13) C63 0.049(2) 0.048(2) 0.055(2) 0.0062(17) 0.0221(19) -0.0067(17) C64 0.0256(16) 0.0368(17) 0.0420(19) 0.0025(15) 0.0103(15) 0.0050(13) C65 0.0377(19) 0.046(2) 0.0395(19) -0.0074(15) 0.0164(16) -0.0028(15) C66 0.0247(16) 0.0483(19) 0.0269(16) -0.0029(14) 0.0084(13) 0.0067(14) C67 0.043(2) 0.066(2) 0.0337(18) -0.0099(16) 0.0167(16) -0.0032(17) C68 0.042(2) 0.051(2) 0.0383(19) 0.0075(15) 0.0180(16) 0.0121(16) C69 0.0387(18) 0.046(2) 0.0219(15) 0.0079(14) 0.0136(14) 0.0058(15) C70 0.048(2) 0.0407(19) 0.0338(18) 0.0044(14) 0.0171(16) 0.0045(16) C71 0.045(2) 0.046(2) 0.0211(16) -0.0031(14) 0.0126(15) -0.0065(16) C72 0.048(2) 0.054(2) 0.041(2) -0.0038(16) 0.0120(17) -0.0115(17) C73 0.0183(14) 0.0350(16) 0.0235(15) -0.0003(12) 0.0091(12) -0.0005(12) C74 0.0210(14) 0.0335(16) 0.0286(15) -0.0042(12) 0.0104(13) -0.0014(12) C75 0.0333(17) 0.0401(18) 0.0340(17) -0.0047(14) 0.0173(15) -0.0025(14) C76 0.042(2) 0.052(2) 0.0372(19) -0.0102(16) 0.0201(16) 0.0002(16) C77 0.044(2) 0.0409(19) 0.048(2) -0.0137(16) 0.0175(17) 0.0043(16) C78 0.0348(18) 0.0356(18) 0.0425(19) -0.0009(14) 0.0127(15) -0.0007(14) C79 0.0167(14) 0.0354(16) 0.0320(16) -0.0018(13) 0.0078(12) -0.0010(12) C80 0.0275(17) 0.052(2) 0.056(2) -0.0014(17) 0.0083(17) -0.0029(15) C81 0.0281(16) 0.0322(16) 0.0357(18) -0.0092(14) 0.0081(14) -0.0013(13) C82 0.0297(17) 0.0444(19) 0.0291(16) 0.0008(14) 0.0043(14) 0.0019(14) C83 0.0368(18) 0.0294(16) 0.0268(16) -0.0017(12) 0.0140(14) 0.0047(13) C84 0.045(2) 0.048(2) 0.0382(19) 0.0118(15) 0.0144(17) 0.0031(16) C101 0.084(4) 0.080(3) 0.084(3) 0.009(3) 0.027(3) -0.010(3) C102 0.098(4) 0.093(4) 0.095(4) 0.016(3) 0.039(3) 0.024(3) C110 0.063(3) 0.070(3) 0.051(2) -0.014(2) 0.017(2) -0.012(2) C777 0.118(5) 0.123(5) 0.070(3) 0.002(3) 0.020(3) 0.046(4) C888 0.090(4) 0.079(3) 0.055(3) -0.022(2) 0.019(3) 0.005(3) C999 0.074(3) 0.073(3) 0.047(2) -0.012(2) 0.023(2) -0.010(2) _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 N2 1.956(2) . ? Ru1 N1 1.977(2) . ? Ru1 O1 2.017(2) . ? Ru1 O2 2.0527(19) . ? Ru1 O4 2.0555(19) . ? Ru1 O3 2.0795(18) . ? Ru2 N3 1.962(2) . ? Ru2 N4 1.964(2) . ? Ru2 O8 1.9971(19) . ? Ru2 O5 2.0541(18) . ? Ru2 O7 2.0612(18) . ? Ru2 O6 2.0752(19) . ? Ru3 N6 1.952(2) . ? Ru3 N5 1.972(2) . ? Ru3 O12 2.017(2) . ? Ru3 O9 2.053(2) . ? Ru3 O11 2.062(2) . ? Ru3 O10 2.0791(18) . ? Ru4 N7 1.960(2) . ? Ru4 N7 1.960(2) 2_655 ? Ru4 O13 2.031(2) 2_655 ? Ru4 O13 2.031(2) . ? Ru4 O14 2.0873(19) 2_655 ? Ru4 O14 2.0873(19) . ? O1 C16 1.274(4) . ? O2 C18 1.267(4) . ? O3 C21 1.270(4) . ? O4 C23 1.273(3) . ? O5 C40 1.279(3) . ? O6 C42 1.271(3) . ? O7 C45 1.267(4) . ? O8 C47 1.276(4) . ? O9 C64 1.277(4) . ? O10 C66 1.262(4) . ? O11 C69 1.270(4) . ? O12 C71 1.280(4) . ? O13 C81 1.268(4) . ? O14 C83 1.274(3) . ? N1 C1 1.315(3) . ? N1 H1N 0.8800 . ? N2 C14 1.322(4) . ? N2 H2N 0.8800 . ? N3 C25 1.325(4) . ? N3 H3N 0.8800 . ? N4 C38 1.312(4) . ? N4 H4N 0.8800 . ? N5 C49 1.319(4) . ? N5 H5N 0.8800 . ? N6 C62 1.320(4) . ? N6 H6N 0.8800 . ? N7 C73 1.310(4) . ? N7 H7N 0.8800 . ? C1 C14 1.444(4) . ? C1 C2 1.450(4) . ? C2 C3 1.408(4) . ? C2 C7 1.414(4) . ? C3 C4 1.368(4) . ? C3 H3 0.9500 . ? C4 C5 1.395(5) . ? C4 H4 0.9500 . ? C5 C6 1.370(5) . ? C5 H5 0.9500 . ? C6 C7 1.408(4) . ? C6 H6 0.9500 . ? C7 C8 1.471(4) . ? C8 C9 1.403(4) . ? C8 C13 1.415(4) . ? C9 C10 1.371(5) . ? C9 H9 0.9500 . ? C10 C11 1.386(5) . ? C10 H10 0.9500 . ? C11 C12 1.377(4) . ? C11 H11 0.9500 . ? C12 C13 1.397(4) . ? C12 H12 0.9500 . ? C13 C14 1.457(4) . ? C15 C16 1.510(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.395(4) . ? C17 C18 1.401(4) . ? C17 H17 0.9500 . ? C18 C19 1.506(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.506(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.383(4) . ? C22 C23 1.393(4) . ? C22 H22 0.9500 . ? C23 C24 1.501(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C38 1.437(4) . ? C25 C26 1.451(4) . ? C26 C27 1.407(4) . ? C26 C31 1.415(4) . ? C27 C28 1.365(4) . ? C27 H27 0.9500 . ? C28 C29 1.386(5) . ? C28 H28 0.9500 . ? C29 C30 1.371(5) . ? C29 H29 0.9500 . ? C30 C31 1.398(4) . ? C30 H30 0.9500 . ? C31 C32 1.472(4) . ? C32 C37 1.403(4) . ? C32 C33 1.410(4) . ? C33 C34 1.367(5) . ? C33 H33 0.9500 . ? C34 C35 1.383(5) . ? C34 H34 0.9500 . ? C35 C36 1.376(4) . ? C35 H35 0.9500 . ? C36 C37 1.397(4) . ? C36 H36 0.9500 . ? C37 C38 1.463(4) . ? C39 C40 1.503(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.390(4) . ? C41 C42 1.396(4) . ? C41 H41 0.9500 . ? C42 C43 1.506(4) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.510(4) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.410(4) . ? C46 C47 1.386(4) . ? C46 H46 0.9500 . ? C47 C48 1.514(4) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C62 1.437(4) . ? C49 C50 1.454(4) . ? C50 C51 1.402(4) . ? C50 C55 1.422(4) . ? C51 C52 1.374(4) . ? C51 H51 0.9500 . ? C52 C53 1.387(5) . ? C52 H52 0.9500 . ? C53 C54 1.370(4) . ? C53 H53 0.9500 . ? C54 C55 1.397(4) . ? C54 H54 0.9500 . ? C55 C56 1.476(4) . ? C56 C61 1.408(4) . ? C56 C57 1.415(4) . ? C57 C58 1.371(5) . ? C57 H57 0.9500 . ? C58 C59 1.384(5) . ? C58 H58 0.9500 . ? C59 C60 1.375(4) . ? C59 H59 0.9500 . ? C60 C61 1.398(4) . ? C60 H60 0.9500 . ? C61 C62 1.456(4) . ? C63 C64 1.503(4) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.390(4) . ? C65 C66 1.392(4) . ? C65 H65 0.9500 . ? C66 C67 1.515(4) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.502(4) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C70 1.399(5) . ? C70 C71 1.394(5) . ? C70 H70 0.9500 . ? C71 C72 1.504(5) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C73 1.451(5) 2_655 ? C73 C74 1.453(4) . ? C74 C75 1.408(4) . ? C74 C79 1.415(4) . ? C75 C76 1.374(4) . ? C75 H75 0.9500 . ? C76 C77 1.383(5) . ? C76 H76 0.9500 . ? C77 C78 1.377(4) . ? C77 H77 0.9500 . ? C78 C79 1.400(4) . ? C78 H78 0.9500 . ? C79 C79 1.477(5) 2_655 ? C80 C81 1.508(4) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C82 1.395(4) . ? C82 C83 1.382(4) . ? C82 H82 0.9500 . ? C83 C84 1.508(4) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C101 C102 1.492(7) . ? C101 C110 1.529(6) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9800 . ? C102 H10D 0.9800 . ? C102 H10E 0.9800 . ? C110 C999 1.493(6) . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C777 C888 1.497(7) . ? C777 H77A 0.9800 . ? C777 H77B 0.9800 . ? C777 H77C 0.9800 . ? C888 C999 1.507(6) . ? C888 H88A 0.9900 . ? C888 H88B 0.9900 . ? C999 H99A 0.9900 . ? C999 H99B 0.9900 . ? 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 N2 Ru1 N1 78.07(9) . . ? N2 Ru1 O1 91.23(9) . . ? N1 Ru1 O1 89.55(9) . . ? N2 Ru1 O2 95.11(9) . . ? N1 Ru1 O2 173.10(8) . . ? O1 Ru1 O2 91.67(8) . . ? N2 Ru1 O4 91.77(8) . . ? N1 Ru1 O4 93.00(9) . . ? O1 Ru1 O4 176.41(8) . . ? O2 Ru1 O4 86.09(8) . . ? N2 Ru1 O3 176.87(8) . . ? N1 Ru1 O3 99.49(9) . . ? O1 Ru1 O3 86.76(8) . . ? O2 Ru1 O3 87.35(8) . . ? O4 Ru1 O3 90.33(8) . . ? N3 Ru2 N4 78.12(9) . . ? N3 Ru2 O8 91.08(9) . . ? N4 Ru2 O8 86.90(8) . . ? N3 Ru2 O5 92.69(8) . . ? N4 Ru2 O5 95.30(8) . . ? O8 Ru2 O5 175.96(8) . . ? N3 Ru2 O7 95.50(8) . . ? N4 Ru2 O7 173.26(9) . . ? O8 Ru2 O7 91.09(8) . . ? O5 Ru2 O7 87.11(7) . . ? N3 Ru2 O6 175.23(8) . . ? N4 Ru2 O6 98.01(8) . . ? O8 Ru2 O6 85.89(8) . . ? O5 Ru2 O6 90.45(7) . . ? O7 Ru2 O6 88.25(7) . . ? N6 Ru3 N5 78.21(10) . . ? N6 Ru3 O12 92.43(9) . . ? N5 Ru3 O12 86.86(9) . . ? N6 Ru3 O9 92.15(9) . . ? N5 Ru3 O9 96.69(9) . . ? O12 Ru3 O9 174.70(8) . . ? N6 Ru3 O11 93.98(9) . . ? N5 Ru3 O11 171.97(9) . . ? O12 Ru3 O11 91.65(8) . . ? O9 Ru3 O11 85.37(8) . . ? N6 Ru3 O10 175.49(9) . . ? N5 Ru3 O10 97.78(9) . . ? O12 Ru3 O10 85.26(8) . . ? O9 Ru3 O10 90.34(8) . . ? O11 Ru3 O10 89.96(8) . . ? N7 Ru4 N7 78.05(13) . 2_655 ? N7 Ru4 O13 86.28(9) . 2_655 ? N7 Ru4 O13 95.81(9) 2_655 2_655 ? N7 Ru4 O13 95.81(9) . . ? N7 Ru4 O13 86.28(9) 2_655 . ? O13 Ru4 O13 177.31(11) 2_655 . ? N7 Ru4 O14 172.68(9) . 2_655 ? N7 Ru4 O14 97.15(8) 2_655 2_655 ? O13 Ru4 O14 88.74(8) 2_655 2_655 ? O13 Ru4 O14 89.33(8) . 2_655 ? N7 Ru4 O14 97.15(8) . . ? N7 Ru4 O14 172.68(9) 2_655 . ? O13 Ru4 O14 89.33(8) 2_655 . ? O13 Ru4 O14 88.74(8) . . ? O14 Ru4 O14 88.14(10) 2_655 . ? C16 O1 Ru1 123.52(19) . . ? C18 O2 Ru1 122.80(19) . . ? C21 O3 Ru1 124.87(18) . . ? C23 O4 Ru1 124.87(18) . . ? C40 O5 Ru2 124.77(17) . . ? C42 O6 Ru2 125.11(17) . . ? C45 O7 Ru2 122.21(18) . . ? C47 O8 Ru2 123.66(18) . . ? C64 O9 Ru3 125.03(18) . . ? C66 O10 Ru3 124.82(18) . . ? C69 O11 Ru3 121.8(2) . . ? C71 O12 Ru3 123.3(2) . . ? C81 O13 Ru4 126.54(18) . . ? C83 O14 Ru4 124.90(18) . . ? C1 N1 Ru1 117.54(19) . . ? C1 N1 H1N 121.2 . . ? Ru1 N1 H1N 121.2 . . ? C14 N2 Ru1 118.18(18) . . ? C14 N2 H2N 120.9 . . ? Ru1 N2 H2N 120.9 . . ? C25 N3 Ru2 117.52(18) . . ? C25 N3 H3N 121.2 . . ? Ru2 N3 H3N 121.2 . . ? C38 N4 Ru2 117.62(18) . . ? C38 N4 H4N 121.2 . . ? Ru2 N4 H4N 121.2 . . ? C49 N5 Ru3 117.01(19) . . ? C49 N5 H5N 121.5 . . ? Ru3 N5 H5N 121.5 . . ? C62 N6 Ru3 117.85(19) . . ? C62 N6 H6N 121.1 . . ? Ru3 N6 H6N 121.1 . . ? C73 N7 Ru4 117.98(17) . . ? C73 N7 H7N 121.0 . . ? Ru4 N7 H7N 121.0 . . ? N1 C1 C14 113.2(2) . . ? N1 C1 C2 126.7(3) . . ? C14 C1 C2 119.9(2) . . ? C3 C2 C7 119.7(3) . . ? C3 C2 C1 121.1(3) . . ? C7 C2 C1 119.2(3) . . ? C4 C3 C2 120.9(3) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 119.8(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 120.3(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 121.5(3) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C6 C7 C2 117.7(3) . . ? C6 C7 C8 121.4(3) . . ? C2 C7 C8 120.8(3) . . ? C9 C8 C13 117.5(3) . . ? C9 C8 C7 122.0(3) . . ? C13 C8 C7 120.5(2) . . ? C10 C9 C8 121.8(3) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C9 C10 C11 120.3(3) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 119.6(3) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 121.0(3) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C8 119.8(3) . . ? C12 C13 C14 121.5(3) . . ? C8 C13 C14 118.7(2) . . ? N2 C14 C1 112.9(2) . . ? N2 C14 C13 126.3(2) . . ? C1 C14 C13 120.8(2) . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O1 C16 C17 126.2(3) . . ? O1 C16 C15 113.8(3) . . ? C17 C16 C15 119.9(3) . . ? C16 C17 C18 127.0(3) . . ? C16 C17 H17 116.5 . . ? C18 C17 H17 116.5 . . ? O2 C18 C17 125.5(3) . . ? O2 C18 C19 115.1(3) . . ? C17 C18 C19 119.4(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O3 C21 C22 125.7(3) . . ? O3 C21 C20 115.2(3) . . ? C22 C21 C20 119.1(3) . . ? C21 C22 C23 127.9(3) . . ? C21 C22 H22 116.0 . . ? C23 C22 H22 116.0 . . ? O4 C23 C22 126.2(3) . . ? O4 C23 C24 114.9(3) . . ? C22 C23 C24 118.9(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C38 112.8(2) . . ? N3 C25 C26 126.4(3) . . ? C38 C25 C26 120.8(2) . . ? C27 C26 C31 119.5(3) . . ? C27 C26 C25 122.1(3) . . ? C31 C26 C25 118.4(3) . . ? C28 C27 C26 120.9(3) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 120.2(3) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 119.7(3) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 122.2(3) . . ? C29 C30 H30 118.9 . . ? C31 C30 H30 118.9 . . ? C30 C31 C26 117.5(3) . . ? C30 C31 C32 121.8(3) . . ? C26 C31 C32 120.7(3) . . ? C37 C32 C33 117.0(3) . . ? C37 C32 C31 121.2(3) . . ? C33 C32 C31 121.8(3) . . ? C34 C33 C32 122.1(3) . . ? C34 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? C33 C34 C35 120.2(3) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 119.6(3) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C35 C36 C37 120.8(3) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C36 C37 C32 120.3(3) . . ? C36 C37 C38 121.4(3) . . ? C32 C37 C38 118.2(3) . . ? N4 C38 C25 113.5(2) . . ? N4 C38 C37 125.9(3) . . ? C25 C38 C37 120.5(3) . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O5 C40 C41 126.5(3) . . ? O5 C40 C39 114.5(3) . . ? C41 C40 C39 119.0(3) . . ? C40 C41 C42 127.4(3) . . ? C40 C41 H41 116.3 . . ? C42 C41 H41 116.3 . . ? O6 C42 C41 125.7(3) . . ? O6 C42 C43 115.4(3) . . ? C41 C42 C43 118.9(3) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 H44A 109.5 . . ? C45 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C45 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O7 C45 C46 125.5(3) . . ? O7 C45 C44 115.6(3) . . ? C46 C45 C44 118.9(3) . . ? C47 C46 C45 126.0(3) . . ? C47 C46 H46 117.0 . . ? C45 C46 H46 117.0 . . ? O8 C47 C46 126.6(3) . . ? O8 C47 C48 112.4(3) . . ? C46 C47 C48 121.0(3) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N5 C49 C62 113.3(3) . . ? N5 C49 C50 126.6(3) . . ? C62 C49 C50 120.1(3) . . ? C51 C50 C55 119.3(3) . . ? C51 C50 C49 121.6(3) . . ? C55 C50 C49 119.2(3) . . ? C52 C51 C50 121.2(3) . . ? C52 C51 H51 119.4 . . ? C50 C51 H51 119.4 . . ? C51 C52 C53 119.3(3) . . ? C51 C52 H52 120.3 . . ? C53 C52 H52 120.3 . . ? C54 C53 C52 120.8(3) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C53 C54 C55 121.5(3) . . ? C53 C54 H54 119.3 . . ? C55 C54 H54 119.3 . . ? C54 C55 C50 117.9(3) . . ? C54 C55 C56 122.0(3) . . ? C50 C55 C56 120.1(3) . . ? C61 C56 C57 117.7(3) . . ? C61 C56 C55 121.0(3) . . ? C57 C56 C55 121.4(3) . . ? C58 C57 C56 121.5(3) . . ? C58 C57 H57 119.2 . . ? C56 C57 H57 119.2 . . ? C57 C58 C59 120.1(3) . . ? C57 C58 H58 120.0 . . ? C59 C58 H58 120.0 . . ? C60 C59 C58 119.9(3) . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C60 C61 121.0(3) . . ? C59 C60 H60 119.5 . . ? C61 C60 H60 119.5 . . ? C60 C61 C56 119.7(3) . . ? C60 C61 C62 121.5(3) . . ? C56 C61 C62 118.8(3) . . ? N6 C62 C49 113.0(2) . . ? N6 C62 C61 126.1(3) . . ? C49 C62 C61 120.8(3) . . ? C64 C63 H63A 109.5 . . ? C64 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C64 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O9 C64 C65 126.0(3) . . ? O9 C64 C63 114.5(3) . . ? C65 C64 C63 119.5(3) . . ? C64 C65 C66 127.6(3) . . ? C64 C65 H65 116.2 . . ? C66 C65 H65 116.2 . . ? O10 C66 C65 126.0(3) . . ? O10 C66 C67 114.1(3) . . ? C65 C66 C67 119.8(3) . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C69 C68 H68A 109.5 . . ? C69 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C69 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O11 C69 C70 125.6(3) . . ? O11 C69 C68 115.5(3) . . ? C70 C69 C68 118.8(3) . . ? C71 C70 C69 127.1(3) . . ? C71 C70 H70 116.5 . . ? C69 C70 H70 116.5 . . ? O12 C71 C70 126.1(3) . . ? O12 C71 C72 114.0(3) . . ? C70 C71 C72 119.9(3) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N7 C73 C73 112.66(15) . 2_655 ? N7 C73 C74 127.3(2) . . ? C73 C73 C74 120.03(15) 2_655 . ? C75 C74 C79 119.4(3) . . ? C75 C74 C73 121.3(3) . . ? C79 C74 C73 119.2(2) . . ? C76 C75 C74 120.6(3) . . ? C76 C75 H75 119.7 . . ? C74 C75 H75 119.7 . . ? C75 C76 C77 120.2(3) . . ? C75 C76 H76 119.9 . . ? C77 C76 H76 119.9 . . ? C78 C77 C76 120.0(3) . . ? C78 C77 H77 120.0 . . ? C76 C77 H77 120.0 . . ? C77 C78 C79 121.7(3) . . ? C77 C78 H78 119.2 . . ? C79 C78 H78 119.2 . . ? C78 C79 C74 117.9(3) . . ? C78 C79 C79 121.72(18) . 2_655 ? C74 C79 C79 120.41(16) . 2_655 ? C81 C80 H80A 109.5 . . ? C81 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C81 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? O13 C81 C82 125.7(3) . . ? O13 C81 C80 114.4(3) . . ? C82 C81 C80 119.9(3) . . ? C83 C82 C81 126.6(3) . . ? C83 C82 H82 116.7 . . ? C81 C82 H82 116.7 . . ? O14 C83 C82 125.6(3) . . ? O14 C83 C84 114.9(3) . . ? C82 C83 C84 119.4(3) . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C102 C101 C110 113.9(4) . . ? C102 C101 H10A 108.8 . . ? C110 C101 H10A 108.8 . . ? C102 C101 H10B 108.8 . . ? C110 C101 H10B 108.8 . . ? H10A C101 H10B 107.7 . . ? C101 C102 H10C 109.5 . . ? C101 C102 H10D 109.5 . . ? H10C C102 H10D 109.5 . . ? C101 C102 H10E 109.5 . . ? H10C C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? C999 C110 C101 115.7(4) . . ? C999 C110 H11A 108.4 . . ? C101 C110 H11A 108.4 . . ? C999 C110 H11B 108.4 . . ? C101 C110 H11B 108.4 . . ? H11A C110 H11B 107.4 . . ? C888 C777 H77A 109.5 . . ? C888 C777 H77B 109.5 . . ? H77A C777 H77B 109.5 . . ? C888 C777 H77C 109.5 . . ? H77A C777 H77C 109.5 . . ? H77B C777 H77C 109.5 . . ? C777 C888 C999 114.0(4) . . ? C777 C888 H88A 108.7 . . ? C999 C888 H88A 108.7 . . ? C777 C888 H88B 108.7 . . ? C999 C888 H88B 108.7 . . ? H88A C888 H88B 107.6 . . ? C110 C999 C888 115.7(4) . . ? C110 C999 H99A 108.4 . . ? C888 C999 H99A 108.4 . . ? C110 C999 H99B 108.4 . . ? C888 C999 H99B 108.4 . . ? H99A C999 H99B 107.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru1 O1 C16 -79.8(2) . . . . ? N1 Ru1 O1 C16 -157.9(2) . . . . ? O2 Ru1 O1 C16 15.3(2) . . . . ? O4 Ru1 O1 C16 66.8(13) . . . . ? O3 Ru1 O1 C16 102.6(2) . . . . ? N2 Ru1 O2 C18 72.3(2) . . . . ? N1 Ru1 O2 C18 81.1(8) . . . . ? O1 Ru1 O2 C18 -19.1(2) . . . . ? O4 Ru1 O2 C18 163.7(2) . . . . ? O3 Ru1 O2 C18 -105.7(2) . . . . ? N2 Ru1 O3 C21 136.0(16) . . . . ? N1 Ru1 O3 C21 97.2(2) . . . . ? O1 Ru1 O3 C21 -173.8(2) . . . . ? O2 Ru1 O3 C21 -82.0(2) . . . . ? O4 Ru1 O3 C21 4.1(2) . . . . ? N2 Ru1 O4 C23 -179.0(2) . . . . ? N1 Ru1 O4 C23 -100.9(2) . . . . ? O1 Ru1 O4 C23 34.4(13) . . . . ? O2 Ru1 O4 C23 86.0(2) . . . . ? O3 Ru1 O4 C23 -1.3(2) . . . . ? N3 Ru2 O5 C40 -176.1(2) . . . . ? N4 Ru2 O5 C40 -97.7(2) . . . . ? O8 Ru2 O5 C40 25.1(12) . . . . ? O7 Ru2 O5 C40 88.6(2) . . . . ? O6 Ru2 O5 C40 0.3(2) . . . . ? N3 Ru2 O6 C42 133.3(10) . . . . ? N4 Ru2 O6 C42 97.6(2) . . . . ? O8 Ru2 O6 C42 -176.1(2) . . . . ? O5 Ru2 O6 C42 2.2(2) . . . . ? O7 Ru2 O6 C42 -84.9(2) . . . . ? N3 Ru2 O7 C45 68.2(2) . . . . ? N4 Ru2 O7 C45 49.6(8) . . . . ? O8 Ru2 O7 C45 -23.0(2) . . . . ? O5 Ru2 O7 C45 160.6(2) . . . . ? O6 Ru2 O7 C45 -108.8(2) . . . . ? N3 Ru2 O8 C47 -76.1(2) . . . . ? N4 Ru2 O8 C47 -154.1(2) . . . . ? O5 Ru2 O8 C47 82.8(11) . . . . ? O7 Ru2 O8 C47 19.4(2) . . . . ? O6 Ru2 O8 C47 107.6(2) . . . . ? N6 Ru3 O9 C64 171.9(2) . . . . ? N5 Ru3 O9 C64 93.6(2) . . . . ? O12 Ru3 O9 C64 -38.2(10) . . . . ? O11 Ru3 O9 C64 -94.2(2) . . . . ? O10 Ru3 O9 C64 -4.3(2) . . . . ? N6 Ru3 O10 C66 -120.6(11) . . . . ? N5 Ru3 O10 C66 -93.7(2) . . . . ? O12 Ru3 O10 C66 -179.9(2) . . . . ? O9 Ru3 O10 C66 3.1(2) . . . . ? O11 Ru3 O10 C66 88.4(2) . . . . ? N6 Ru3 O11 C69 -70.3(2) . . . . ? N5 Ru3 O11 C69 -56.9(7) . . . . ? O12 Ru3 O11 C69 22.3(2) . . . . ? O9 Ru3 O11 C69 -162.1(2) . . . . ? O10 Ru3 O11 C69 107.6(2) . . . . ? N6 Ru3 O12 C71 78.0(2) . . . . ? N5 Ru3 O12 C71 156.1(2) . . . . ? O9 Ru3 O12 C71 -71.8(9) . . . . ? O11 Ru3 O12 C71 -16.0(2) . . . . ? O10 Ru3 O12 C71 -105.8(2) . . . . ? N7 Ru4 O13 C81 -84.6(2) . . . . ? N7 Ru4 O13 C81 -162.2(2) 2_655 . . . ? O13 Ru4 O13 C81 56.5(2) 2_655 . . . ? O14 Ru4 O13 C81 100.6(2) 2_655 . . . ? O14 Ru4 O13 C81 12.4(2) . . . . ? N7 Ru4 O14 C83 82.0(2) . . . . ? N7 Ru4 O14 C83 33.5(7) 2_655 . . . ? O13 Ru4 O14 C83 168.2(2) 2_655 . . . ? O13 Ru4 O14 C83 -13.7(2) . . . . ? O14 Ru4 O14 C83 -103.0(2) 2_655 . . . ? N2 Ru1 N1 C1 -2.2(2) . . . . ? O1 Ru1 N1 C1 89.2(2) . . . . ? O2 Ru1 N1 C1 -11.1(9) . . . . ? O4 Ru1 N1 C1 -93.4(2) . . . . ? O3 Ru1 N1 C1 175.80(19) . . . . ? N1 Ru1 N2 C14 2.6(2) . . . . ? O1 Ru1 N2 C14 -86.6(2) . . . . ? O2 Ru1 N2 C14 -178.4(2) . . . . ? O4 Ru1 N2 C14 95.3(2) . . . . ? O3 Ru1 N2 C14 -36.6(17) . . . . ? N4 Ru2 N3 C25 5.29(19) . . . . ? O8 Ru2 N3 C25 -81.3(2) . . . . ? O5 Ru2 N3 C25 100.1(2) . . . . ? O7 Ru2 N3 C25 -172.51(19) . . . . ? O6 Ru2 N3 C25 -30.9(11) . . . . ? N3 Ru2 N4 C38 -5.63(19) . . . . ? O8 Ru2 N4 C38 86.1(2) . . . . ? O5 Ru2 N4 C38 -97.3(2) . . . . ? O7 Ru2 N4 C38 13.4(8) . . . . ? O6 Ru2 N4 C38 171.52(19) . . . . ? N6 Ru3 N5 C49 7.3(2) . . . . ? O12 Ru3 N5 C49 -85.9(2) . . . . ? O9 Ru3 N5 C49 98.1(2) . . . . ? O11 Ru3 N5 C49 -6.4(8) . . . . ? O10 Ru3 N5 C49 -170.7(2) . . . . ? N5 Ru3 N6 C62 -6.5(2) . . . . ? O12 Ru3 N6 C62 79.7(2) . . . . ? O9 Ru3 N6 C62 -102.9(2) . . . . ? O11 Ru3 N6 C62 171.6(2) . . . . ? O10 Ru3 N6 C62 20.7(13) . . . . ? N7 Ru4 N7 C73 -2.79(15) 2_655 . . . ? O13 Ru4 N7 C73 94.0(2) 2_655 . . . ? O13 Ru4 N7 C73 -87.7(2) . . . . ? O14 Ru4 N7 C73 46.7(7) 2_655 . . . ? O14 Ru4 N7 C73 -177.2(2) . . . . ? Ru1 N1 C1 C14 1.4(3) . . . . ? Ru1 N1 C1 C2 177.3(2) . . . . ? N1 C1 C2 C3 -0.8(4) . . . . ? C14 C1 C2 C3 174.8(3) . . . . ? N1 C1 C2 C7 -178.4(3) . . . . ? C14 C1 C2 C7 -2.8(4) . . . . ? C7 C2 C3 C4 0.7(4) . . . . ? C1 C2 C3 C4 -176.9(3) . . . . ? C2 C3 C4 C5 -1.1(5) . . . . ? C3 C4 C5 C6 0.6(5) . . . . ? C4 C5 C6 C7 0.3(5) . . . . ? C5 C6 C7 C2 -0.7(5) . . . . ? C5 C6 C7 C8 178.0(3) . . . . ? C3 C2 C7 C6 0.2(4) . . . . ? C1 C2 C7 C6 177.8(3) . . . . ? C3 C2 C7 C8 -178.5(3) . . . . ? C1 C2 C7 C8 -0.9(4) . . . . ? C6 C7 C8 C9 3.6(4) . . . . ? C2 C7 C8 C9 -177.8(3) . . . . ? C6 C7 C8 C13 -174.9(3) . . . . ? C2 C7 C8 C13 3.8(4) . . . . ? C13 C8 C9 C10 1.0(5) . . . . ? C7 C8 C9 C10 -177.6(3) . . . . ? C8 C9 C10 C11 -0.8(6) . . . . ? C9 C10 C11 C12 0.7(6) . . . . ? C10 C11 C12 C13 -0.9(5) . . . . ? C11 C12 C13 C8 1.1(4) . . . . ? C11 C12 C13 C14 -178.7(3) . . . . ? C9 C8 C13 C12 -1.1(4) . . . . ? C7 C8 C13 C12 177.5(3) . . . . ? C9 C8 C13 C14 178.7(3) . . . . ? C7 C8 C13 C14 -2.8(4) . . . . ? Ru1 N2 C14 C1 -2.6(3) . . . . ? Ru1 N2 C14 C13 178.2(2) . . . . ? N1 C1 C14 N2 0.7(3) . . . . ? C2 C1 C14 N2 -175.4(2) . . . . ? N1 C1 C14 C13 179.9(2) . . . . ? C2 C1 C14 C13 3.7(4) . . . . ? C12 C13 C14 N2 -2.1(4) . . . . ? C8 C13 C14 N2 178.2(3) . . . . ? C12 C13 C14 C1 178.8(3) . . . . ? C8 C13 C14 C1 -0.9(4) . . . . ? Ru1 O1 C16 C17 -6.9(4) . . . . ? Ru1 O1 C16 C15 172.98(19) . . . . ? O1 C16 C17 C18 -5.2(5) . . . . ? C15 C16 C17 C18 174.9(3) . . . . ? Ru1 O2 C18 C17 14.6(4) . . . . ? Ru1 O2 C18 C19 -165.71(18) . . . . ? C16 C17 C18 O2 0.6(5) . . . . ? C16 C17 C18 C19 -179.1(3) . . . . ? Ru1 O3 C21 C22 -4.9(4) . . . . ? Ru1 O3 C21 C20 175.8(2) . . . . ? O3 C21 C22 C23 2.0(6) . . . . ? C20 C21 C22 C23 -178.8(3) . . . . ? Ru1 O4 C23 C22 -0.8(4) . . . . ? Ru1 O4 C23 C24 178.3(2) . . . . ? C21 C22 C23 O4 1.3(6) . . . . ? C21 C22 C23 C24 -177.8(3) . . . . ? Ru2 N3 C25 C38 -4.2(3) . . . . ? Ru2 N3 C25 C26 176.5(2) . . . . ? N3 C25 C26 C27 -1.3(4) . . . . ? C38 C25 C26 C27 179.5(3) . . . . ? N3 C25 C26 C31 178.3(3) . . . . ? C38 C25 C26 C31 -0.9(4) . . . . ? C31 C26 C27 C28 0.5(4) . . . . ? C25 C26 C27 C28 -179.9(3) . . . . ? C26 C27 C28 C29 1.4(5) . . . . ? C27 C28 C29 C30 -1.2(5) . . . . ? C28 C29 C30 C31 -0.9(5) . . . . ? C29 C30 C31 C26 2.8(5) . . . . ? C29 C30 C31 C32 -175.9(3) . . . . ? C27 C26 C31 C30 -2.5(4) . . . . ? C25 C26 C31 C30 177.9(3) . . . . ? C27 C26 C31 C32 176.2(3) . . . . ? C25 C26 C31 C32 -3.4(4) . . . . ? C30 C31 C32 C37 -175.4(3) . . . . ? C26 C31 C32 C37 6.0(4) . . . . ? C30 C31 C32 C33 7.3(5) . . . . ? C26 C31 C32 C33 -171.4(3) . . . . ? C37 C32 C33 C34 1.0(5) . . . . ? C31 C32 C33 C34 178.4(3) . . . . ? C32 C33 C34 C35 1.6(5) . . . . ? C33 C34 C35 C36 -2.3(5) . . . . ? C34 C35 C36 C37 0.3(5) . . . . ? C35 C36 C37 C32 2.3(4) . . . . ? C35 C36 C37 C38 -174.1(3) . . . . ? C33 C32 C37 C36 -2.9(4) . . . . ? C31 C32 C37 C36 179.6(3) . . . . ? C33 C32 C37 C38 173.6(3) . . . . ? C31 C32 C37 C38 -3.9(4) . . . . ? Ru2 N4 C38 C25 5.1(3) . . . . ? Ru2 N4 C38 C37 -179.4(2) . . . . ? N3 C25 C38 N4 -0.6(3) . . . . ? C26 C25 C38 N4 178.8(2) . . . . ? N3 C25 C38 C37 -176.4(2) . . . . ? C26 C25 C38 C37 3.0(4) . . . . ? C36 C37 C38 N4 0.7(4) . . . . ? C32 C37 C38 N4 -175.8(3) . . . . ? C36 C37 C38 C25 176.0(3) . . . . ? C32 C37 C38 C25 -0.5(4) . . . . ? Ru2 O5 C40 C41 -2.8(4) . . . . ? Ru2 O5 C40 C39 175.97(18) . . . . ? O5 C40 C41 C42 3.3(5) . . . . ? C39 C40 C41 C42 -175.4(3) . . . . ? Ru2 O6 C42 C41 -2.6(4) . . . . ? Ru2 O6 C42 C43 178.78(19) . . . . ? C40 C41 C42 O6 -0.2(5) . . . . ? C40 C41 C42 C43 178.4(3) . . . . ? Ru2 O7 C45 C46 16.2(4) . . . . ? Ru2 O7 C45 C44 -164.49(19) . . . . ? O7 C45 C46 C47 2.6(5) . . . . ? C44 C45 C46 C47 -176.6(3) . . . . ? Ru2 O8 C47 C46 -8.9(5) . . . . ? Ru2 O8 C47 C48 171.6(2) . . . . ? C45 C46 C47 O8 -7.2(6) . . . . ? C45 C46 C47 C48 172.3(3) . . . . ? Ru3 N5 C49 C62 -6.8(3) . . . . ? Ru3 N5 C49 C50 173.7(2) . . . . ? N5 C49 C50 C51 1.2(5) . . . . ? C62 C49 C50 C51 -178.3(3) . . . . ? N5 C49 C50 C55 -179.5(3) . . . . ? C62 C49 C50 C55 1.0(4) . . . . ? C55 C50 C51 C52 1.6(4) . . . . ? C49 C50 C51 C52 -179.2(3) . . . . ? C50 C51 C52 C53 0.1(5) . . . . ? C51 C52 C53 C54 -0.9(5) . . . . ? C52 C53 C54 C55 0.0(5) . . . . ? C53 C54 C55 C50 1.6(5) . . . . ? C53 C54 C55 C56 -177.6(3) . . . . ? C51 C50 C55 C54 -2.4(4) . . . . ? C49 C50 C55 C54 178.3(3) . . . . ? C51 C50 C55 C56 176.8(3) . . . . ? C49 C50 C55 C56 -2.4(4) . . . . ? C54 C55 C56 C61 -179.7(3) . . . . ? C50 C55 C56 C61 1.1(4) . . . . ? C54 C55 C56 C57 1.2(5) . . . . ? C50 C55 C56 C57 -178.0(3) . . . . ? C61 C56 C57 C58 1.0(5) . . . . ? C55 C56 C57 C58 -179.8(3) . . . . ? C56 C57 C58 C59 -0.4(5) . . . . ? C57 C58 C59 C60 -1.3(5) . . . . ? C58 C59 C60 C61 2.3(5) . . . . ? C59 C60 C61 C56 -1.7(5) . . . . ? C59 C60 C61 C62 177.5(3) . . . . ? C57 C56 C61 C60 0.0(4) . . . . ? C55 C56 C61 C60 -179.2(3) . . . . ? C57 C56 C61 C62 -179.1(3) . . . . ? C55 C56 C61 C62 1.7(4) . . . . ? Ru3 N6 C62 C49 4.9(3) . . . . ? Ru3 N6 C62 C61 -176.2(2) . . . . ? N5 C49 C62 N6 1.3(4) . . . . ? C50 C49 C62 N6 -179.1(3) . . . . ? N5 C49 C62 C61 -177.7(3) . . . . ? C50 C49 C62 C61 1.9(4) . . . . ? C60 C61 C62 N6 -1.2(5) . . . . ? C56 C61 C62 N6 178.0(3) . . . . ? C60 C61 C62 C49 177.7(3) . . . . ? C56 C61 C62 C49 -3.2(4) . . . . ? Ru3 O9 C64 C65 3.4(4) . . . . ? Ru3 O9 C64 C63 -178.2(2) . . . . ? O9 C64 C65 C66 0.4(6) . . . . ? C63 C64 C65 C66 -177.8(3) . . . . ? Ru3 O10 C66 C65 -0.8(4) . . . . ? Ru3 O10 C66 C67 -178.5(2) . . . . ? C64 C65 C66 O10 -1.9(6) . . . . ? C64 C65 C66 C67 175.7(3) . . . . ? Ru3 O11 C69 C70 -17.9(4) . . . . ? Ru3 O11 C69 C68 162.66(19) . . . . ? O11 C69 C70 C71 -0.6(5) . . . . ? C68 C69 C70 C71 178.8(3) . . . . ? Ru3 O12 C71 C70 4.7(4) . . . . ? Ru3 O12 C71 C72 -177.00(19) . . . . ? C69 C70 C71 O12 8.5(5) . . . . ? C69 C70 C71 C72 -169.7(3) . . . . ? Ru4 N7 C73 C73 7.2(4) . . . 2_655 ? Ru4 N7 C73 C74 -173.3(2) . . . . ? N7 C73 C74 C75 7.0(5) . . . . ? C73 C73 C74 C75 -173.5(3) 2_655 . . . ? N7 C73 C74 C79 -172.2(3) . . . . ? C73 C73 C74 C79 7.3(5) 2_655 . . . ? C79 C74 C75 C76 2.6(5) . . . . ? C73 C74 C75 C76 -176.6(3) . . . . ? C74 C75 C76 C77 2.1(5) . . . . ? C75 C76 C77 C78 -3.8(5) . . . . ? C76 C77 C78 C79 0.7(5) . . . . ? C77 C78 C79 C74 3.8(5) . . . . ? C77 C78 C79 C79 -176.9(3) . . . 2_655 ? C75 C74 C79 C78 -5.4(4) . . . . ? C73 C74 C79 C78 173.8(3) . . . . ? C75 C74 C79 C79 175.3(3) . . . 2_655 ? C73 C74 C79 C79 -5.5(5) . . . 2_655 ? Ru4 O13 C81 C82 -5.6(4) . . . . ? Ru4 O13 C81 C80 175.4(2) . . . . ? O13 C81 C82 C83 -6.3(5) . . . . ? C80 C81 C82 C83 172.6(3) . . . . ? Ru4 O14 C83 C82 8.3(4) . . . . ? Ru4 O14 C83 C84 -173.48(19) . . . . ? C81 C82 C83 O14 4.6(5) . . . . ? C81 C82 C83 C84 -173.6(3) . . . . ? C102 C101 C110 C999 -177.4(4) . . . . ? C101 C110 C999 C888 175.4(4) . . . . ? C777 C888 C999 C110 177.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.816 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.066 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.232 0.750 543 68 ' ' 2 1.000 0.268 0.250 543 68 ' ' 3 0.000 0.732 0.750 543 68 ' ' 4 0.500 0.768 0.250 543 68 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 963959' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H46 N2 O10 Ru2' _chemical_formula_weight 1013.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.7929(2) _cell_length_b 14.64720(10) _cell_length_c 19.3765(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.8360(10) _cell_angle_gamma 90.00 _cell_volume 4392.45(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 22485 _cell_measurement_theta_min 2.9711 _cell_measurement_theta_max 32.4164 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_T_min 0.7848 _exptl_absorpt_correction_T_max 0.8407 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Micro-Focus (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION SUPER NOVA' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39967 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_unetI/netI 0.0237 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7715 _reflns_number_gt 6905 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0278P)^2^+2.9555P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7715 _refine_ls_number_parameters 567 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0616 _refine_ls_wR_factor_gt 0.0598 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _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 0.800726(11) 0.316584(12) 0.667735(10) 0.02178(6) Uani 1 1 d . . . Ru2 Ru 0.748198(11) 0.020380(12) 0.775997(9) 0.02070(6) Uani 1 1 d . . . O1 O 0.69590(10) 0.35134(11) 0.57420(8) 0.0258(3) Uani 1 1 d . . . O2 O 0.89569(10) 0.27398(11) 0.76349(8) 0.0269(4) Uani 1 1 d . . . O3 O 0.79854(10) 0.44323(11) 0.70705(8) 0.0266(4) Uani 1 1 d . . . O4 O 0.89436(10) 0.36656(11) 0.63292(8) 0.0272(4) Uani 1 1 d . . . O5 O 0.81005(10) 0.19139(10) 0.62414(8) 0.0258(3) Uani 1 1 d . . . O6 O 0.62202(10) 0.00001(10) 0.75455(8) 0.0240(3) Uani 1 1 d . . . O7 O 0.79513(10) -0.04453(11) 0.87830(9) 0.0277(4) Uani 1 1 d . . . O8 O 0.74490(9) 0.14230(11) 0.82556(8) 0.0239(3) Uani 1 1 d . . . O9 O 0.87093(9) 0.05299(11) 0.79232(8) 0.0251(3) Uani 1 1 d . . . O10 O 0.75558(10) -0.10322(11) 0.73269(9) 0.0288(4) Uani 1 1 d . . . N1 N 0.70718(12) 0.27886(12) 0.69600(10) 0.0214(4) Uani 1 1 d . . . H1 H 0.7171 0.2468 0.7369 0.026 Uiso 1 1 calc R . . N2 N 0.69526(11) 0.07421(12) 0.67683(9) 0.0199(4) Uani 1 1 d . . . H2 H 0.7265 0.1007 0.6551 0.024 Uiso 1 1 calc R . . C1 C 0.62721(14) 0.30311(14) 0.65141(12) 0.0210(5) Uani 1 1 d . . . C2 C 0.54870(14) 0.28979(15) 0.66462(12) 0.0222(5) Uani 1 1 d . . . C3 C 0.54921(15) 0.24826(15) 0.72995(12) 0.0248(5) Uani 1 1 d . . . H3 H 0.6016 0.2236 0.7650 0.030 Uiso 1 1 calc R . . C4 C 0.47525(16) 0.24249(17) 0.74444(14) 0.0307(5) Uani 1 1 d . . . H4 H 0.4766 0.2132 0.7886 0.037 Uiso 1 1 calc R . . C5 C 0.39885(16) 0.27975(18) 0.69414(15) 0.0362(6) Uani 1 1 d . . . H5 H 0.3486 0.2795 0.7054 0.043 Uiso 1 1 calc R . . C6 C 0.39581(15) 0.31707(17) 0.62817(14) 0.0330(6) Uani 1 1 d . . . H6 H 0.3426 0.3406 0.5936 0.040 Uiso 1 1 calc R . . C7 C 0.46944(15) 0.32145(15) 0.61034(13) 0.0248(5) Uani 1 1 d . . . C8 C 0.46603(15) 0.35702(15) 0.53827(13) 0.0266(5) Uani 1 1 d . . . C9 C 0.38749(16) 0.37905(17) 0.47944(14) 0.0340(6) Uani 1 1 d . . . H9 H 0.3350 0.3715 0.4865 0.041 Uiso 1 1 calc R . . C10 C 0.38481(18) 0.41123(17) 0.41202(14) 0.0395(6) Uani 1 1 d . . . H10 H 0.3308 0.4261 0.3735 0.047 Uiso 1 1 calc R . . C11 C 0.46028(18) 0.42217(16) 0.39966(13) 0.0366(6) Uani 1 1 d . . . H11 H 0.4578 0.4440 0.3527 0.044 Uiso 1 1 calc R . . C12 C 0.53885(17) 0.40124(15) 0.45569(13) 0.0291(5) Uani 1 1 d . . . H12 H 0.5906 0.4090 0.4474 0.035 Uiso 1 1 calc R . . C13 C 0.54240(15) 0.36850(15) 0.52494(12) 0.0246(5) Uani 1 1 d . . . C14 C 0.62414(14) 0.34362(15) 0.58312(12) 0.0219(5) Uani 1 1 d . . . C15 C 0.97350(18) 0.2648(2) 0.89296(14) 0.0440(7) Uani 1 1 d . . . H15A H 0.9499 0.2036 0.8928 0.066 Uiso 1 1 calc R . . H15B H 0.9772 0.2974 0.9383 0.066 Uiso 1 1 calc R . . H15C H 1.0313 0.2598 0.8921 0.066 Uiso 1 1 calc R . . C16 C 0.91520(15) 0.31653(17) 0.82480(13) 0.0286(5) Uani 1 1 d . . . C17 C 0.88904(16) 0.40554(17) 0.83282(13) 0.0309(5) Uani 1 1 d . . . H17 H 0.9076 0.4282 0.8825 0.037 Uiso 1 1 calc R . . C18 C 0.83895(15) 0.46444(16) 0.77620(13) 0.0270(5) Uani 1 1 d . . . C19 C 0.83031(18) 0.56351(17) 0.79356(15) 0.0371(6) Uani 1 1 d . . . H19A H 0.8549 0.6021 0.7655 0.056 Uiso 1 1 calc R . . H19B H 0.8614 0.5742 0.8473 0.056 Uiso 1 1 calc R . . H19C H 0.7691 0.5785 0.7792 0.056 Uiso 1 1 calc R . . C20 C 1.00231(17) 0.37134(19) 0.58299(14) 0.0393(6) Uani 1 1 d . . . H20A H 0.9822 0.3713 0.5283 0.059 Uiso 1 1 calc R . . H20B H 1.0591 0.3419 0.6047 0.059 Uiso 1 1 calc R . . H20C H 1.0069 0.4344 0.6010 0.059 Uiso 1 1 calc R . . C21 C 0.93901(15) 0.31980(17) 0.60602(12) 0.0281(5) Uani 1 1 d . . . C22 C 0.93054(15) 0.22558(18) 0.59272(13) 0.0313(6) Uani 1 1 d . . . H22 H 0.9725 0.1976 0.5779 0.038 Uiso 1 1 calc R . . C23 C 0.86761(15) 0.16890(16) 0.59883(12) 0.0266(5) Uani 1 1 d . . . C24 C 0.85978(18) 0.07253(18) 0.56964(14) 0.0367(6) Uani 1 1 d . . . H24A H 0.8472 0.0313 0.6039 0.055 Uiso 1 1 calc R . . H24B H 0.9142 0.0543 0.5660 0.055 Uiso 1 1 calc R . . H24C H 0.8129 0.0693 0.5200 0.055 Uiso 1 1 calc R . . C25 C 0.60976(14) 0.06921(14) 0.64331(11) 0.0192(4) Uani 1 1 d . . . C26 C 0.55617(14) 0.10107(14) 0.56841(11) 0.0198(4) Uani 1 1 d . . . C27 C 0.59243(15) 0.13665(15) 0.51971(12) 0.0231(5) Uani 1 1 d . . . H27 H 0.6534 0.1424 0.5364 0.028 Uiso 1 1 calc R . . C28 C 0.54072(15) 0.16323(15) 0.44825(12) 0.0252(5) Uani 1 1 d . . . H28 H 0.5661 0.1868 0.4159 0.030 Uiso 1 1 calc R . . C29 C 0.45135(15) 0.15579(15) 0.42316(12) 0.0265(5) Uani 1 1 d . . . H29 H 0.4157 0.1742 0.3738 0.032 Uiso 1 1 calc R . . C30 C 0.41479(15) 0.12155(15) 0.47038(12) 0.0250(5) Uani 1 1 d . . . H30 H 0.3537 0.1166 0.4528 0.030 Uiso 1 1 calc R . . C31 C 0.46543(14) 0.09375(14) 0.54371(12) 0.0204(5) Uani 1 1 d . . . C32 C 0.42613(14) 0.05420(14) 0.59303(12) 0.0215(5) Uani 1 1 d . . . C33 C 0.33657(15) 0.04576(17) 0.57147(13) 0.0286(5) Uani 1 1 d . . . H33 H 0.2991 0.0700 0.5246 0.034 Uiso 1 1 calc R . . C34 C 0.30155(16) 0.00311(18) 0.61654(14) 0.0328(6) Uani 1 1 d . . . H34 H 0.2406 -0.0022 0.6001 0.039 Uiso 1 1 calc R . . C35 C 0.35459(16) -0.03240(17) 0.68616(13) 0.0303(5) Uani 1 1 d . . . H35 H 0.3301 -0.0619 0.7169 0.036 Uiso 1 1 calc R . . C36 C 0.44243(15) -0.02416(15) 0.70954(13) 0.0241(5) Uani 1 1 d . . . H36 H 0.4790 -0.0480 0.7568 0.029 Uiso 1 1 calc R . . C37 C 0.47867(14) 0.01934(14) 0.66398(12) 0.0202(5) Uani 1 1 d . . . C38 C 0.57116(14) 0.02729(14) 0.68926(12) 0.0198(5) Uani 1 1 d . . . C39 C 0.83454(17) -0.0689(2) 1.00763(14) 0.0389(6) Uani 1 1 d . . . H39A H 0.8128 -0.1312 0.9941 0.058 Uiso 1 1 calc R . . H39B H 0.8157 -0.0454 1.0462 0.058 Uiso 1 1 calc R . . H39C H 0.8978 -0.0693 1.0270 0.058 Uiso 1 1 calc R . . C40 C 0.79953(14) -0.00839(17) 0.93899(13) 0.0280(5) Uani 1 1 d . . . C41 C 0.77774(16) 0.08172(18) 0.94802(13) 0.0322(6) Uani 1 1 d . . . H41 H 0.7786 0.0975 0.9959 0.039 Uiso 1 1 calc R . . C42 C 0.75512(14) 0.15027(17) 0.89485(12) 0.0265(5) Uani 1 1 d . . . C43 C 0.74257(17) 0.24627(18) 0.91753(13) 0.0359(6) Uani 1 1 d . . . H43A H 0.7925 0.2838 0.9215 0.054 Uiso 1 1 calc R . . H43B H 0.7371 0.2448 0.9661 0.054 Uiso 1 1 calc R . . H43C H 0.6900 0.2725 0.8797 0.054 Uiso 1 1 calc R . . C44 C 0.99878(16) 0.05390(19) 0.77014(15) 0.0367(6) Uani 1 1 d . . . H44A H 0.9951 0.1200 0.7762 0.055 Uiso 1 1 calc R . . H44B H 1.0105 0.0414 0.7253 0.055 Uiso 1 1 calc R . . H44C H 1.0456 0.0288 0.8142 0.055 Uiso 1 1 calc R . . C45 C 0.91452(15) 0.01004(16) 0.76216(13) 0.0274(5) Uani 1 1 d . . . C46 C 0.89104(16) -0.07414(17) 0.72447(13) 0.0327(6) Uani 1 1 d . . . H46 H 0.9295 -0.0982 0.7038 0.039 Uiso 1 1 calc R . . C47 C 0.81809(16) -0.12567(16) 0.71426(13) 0.0298(5) Uani 1 1 d . . . C48 C 0.8083(2) -0.21868(19) 0.67766(17) 0.0477(7) Uani 1 1 d . . . H48A H 0.7749 -0.2587 0.6969 0.072 Uiso 1 1 calc R . . H48B H 0.8656 -0.2453 0.6891 0.072 Uiso 1 1 calc R . . H48C H 0.7783 -0.2122 0.6233 0.072 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 Ru1 0.02013(10) 0.02580(10) 0.02051(10) 0.00142(7) 0.00910(8) -0.00118(7) Ru2 0.01904(10) 0.02446(10) 0.01899(10) 0.00124(7) 0.00781(7) 0.00268(7) O1 0.0261(9) 0.0310(9) 0.0216(8) 0.0029(7) 0.0106(7) -0.0014(7) O2 0.0233(8) 0.0321(9) 0.0253(8) 0.0035(7) 0.0095(7) 0.0022(7) O3 0.0272(9) 0.0270(8) 0.0273(9) 0.0031(7) 0.0125(7) -0.0002(7) O4 0.0262(9) 0.0335(9) 0.0235(8) -0.0024(7) 0.0114(7) -0.0067(7) O5 0.0244(8) 0.0290(9) 0.0254(8) -0.0008(7) 0.0110(7) -0.0030(7) O6 0.0233(8) 0.0278(8) 0.0216(8) 0.0028(7) 0.0093(7) 0.0008(7) O7 0.0238(8) 0.0325(9) 0.0258(9) 0.0054(7) 0.0085(7) 0.0044(7) O8 0.0229(8) 0.0295(9) 0.0196(8) 0.0000(7) 0.0086(6) 0.0042(7) O9 0.0204(8) 0.0301(9) 0.0246(8) 0.0022(7) 0.0084(7) 0.0041(7) O10 0.0306(9) 0.0256(9) 0.0306(9) 0.0005(7) 0.0124(7) 0.0015(7) N1 0.0245(10) 0.0220(9) 0.0185(9) 0.0006(8) 0.0093(8) 0.0006(8) N2 0.0204(9) 0.0216(9) 0.0207(9) -0.0010(8) 0.0112(8) 0.0001(8) C1 0.0254(12) 0.0156(10) 0.0213(11) -0.0039(9) 0.0085(9) -0.0014(9) C2 0.0253(12) 0.0176(11) 0.0245(11) -0.0067(9) 0.0105(10) -0.0016(9) C3 0.0270(12) 0.0229(12) 0.0253(12) -0.0047(10) 0.0110(10) -0.0007(10) C4 0.0342(14) 0.0319(13) 0.0323(13) -0.0058(11) 0.0197(11) -0.0043(11) C5 0.0292(14) 0.0418(15) 0.0453(15) -0.0090(13) 0.0228(12) -0.0043(12) C6 0.0201(12) 0.0366(14) 0.0398(15) -0.0073(12) 0.0087(11) 0.0028(11) C7 0.0238(12) 0.0189(11) 0.0292(12) -0.0066(10) 0.0076(10) 0.0003(9) C8 0.0273(12) 0.0196(11) 0.0276(12) -0.0060(10) 0.0048(10) 0.0018(10) C9 0.0270(13) 0.0310(13) 0.0354(14) -0.0014(11) 0.0025(11) 0.0026(11) C10 0.0369(15) 0.0311(14) 0.0342(14) -0.0006(12) -0.0042(12) 0.0046(12) C11 0.0533(17) 0.0234(13) 0.0222(12) 0.0033(11) 0.0026(12) 0.0028(12) C12 0.0382(14) 0.0207(12) 0.0258(12) -0.0012(10) 0.0095(11) 0.0003(10) C13 0.0302(13) 0.0175(11) 0.0219(11) -0.0033(9) 0.0056(10) 0.0008(10) C14 0.0264(12) 0.0191(11) 0.0211(11) -0.0037(9) 0.0102(9) -0.0008(9) C15 0.0449(16) 0.0551(18) 0.0273(14) 0.0067(13) 0.0089(12) 0.0092(14) C16 0.0229(12) 0.0401(14) 0.0250(12) 0.0036(11) 0.0116(10) -0.0008(11) C17 0.0306(13) 0.0391(14) 0.0241(12) -0.0037(11) 0.0119(10) -0.0039(11) C18 0.0236(12) 0.0316(13) 0.0315(13) -0.0024(11) 0.0169(11) -0.0053(10) C19 0.0415(15) 0.0320(14) 0.0441(15) -0.0042(12) 0.0236(13) -0.0024(12) C20 0.0335(14) 0.0527(17) 0.0369(14) -0.0102(13) 0.0195(12) -0.0161(13) C21 0.0220(12) 0.0429(15) 0.0181(11) -0.0030(10) 0.0064(9) -0.0072(11) C22 0.0259(13) 0.0427(15) 0.0292(13) -0.0027(11) 0.0150(10) 0.0016(11) C23 0.0247(12) 0.0356(13) 0.0174(11) 0.0005(10) 0.0061(9) 0.0021(10) C24 0.0435(16) 0.0373(14) 0.0324(14) -0.0022(12) 0.0180(12) 0.0023(12) C25 0.0238(11) 0.0166(10) 0.0192(11) -0.0050(9) 0.0105(9) -0.0007(9) C26 0.0251(11) 0.0161(10) 0.0181(10) -0.0039(9) 0.0083(9) -0.0013(9) C27 0.0267(12) 0.0210(11) 0.0227(11) -0.0036(9) 0.0110(10) -0.0022(10) C28 0.0359(13) 0.0222(11) 0.0208(11) -0.0015(10) 0.0146(10) -0.0030(10) C29 0.0342(13) 0.0228(11) 0.0187(11) -0.0006(10) 0.0062(10) 0.0005(10) C30 0.0248(12) 0.0236(12) 0.0243(12) -0.0029(10) 0.0068(10) 0.0007(10) C31 0.0266(12) 0.0148(10) 0.0201(11) -0.0054(9) 0.0096(9) -0.0009(9) C32 0.0247(12) 0.0176(11) 0.0235(11) -0.0051(9) 0.0108(10) -0.0014(9) C33 0.0237(12) 0.0369(14) 0.0237(12) -0.0024(11) 0.0076(10) 0.0001(11) C34 0.0225(12) 0.0446(15) 0.0334(14) -0.0053(12) 0.0130(11) -0.0053(11) C35 0.0308(13) 0.0345(13) 0.0317(13) -0.0019(11) 0.0188(11) -0.0041(11) C36 0.0280(12) 0.0233(12) 0.0239(12) -0.0027(10) 0.0132(10) -0.0011(10) C37 0.0229(11) 0.0169(11) 0.0223(11) -0.0046(9) 0.0103(9) -0.0006(9) C38 0.0252(12) 0.0173(11) 0.0181(11) -0.0029(9) 0.0097(9) 0.0001(9) C39 0.0311(14) 0.0526(17) 0.0282(13) 0.0116(13) 0.0063(11) -0.0005(13) C40 0.0165(11) 0.0415(14) 0.0246(12) 0.0049(11) 0.0065(9) -0.0005(10) C41 0.0305(13) 0.0468(15) 0.0196(11) -0.0008(11) 0.0099(10) 0.0052(12) C42 0.0163(11) 0.0391(14) 0.0220(12) -0.0043(11) 0.0053(9) 0.0023(10) C43 0.0359(14) 0.0417(15) 0.0270(13) -0.0079(12) 0.0090(11) 0.0070(12) C44 0.0254(13) 0.0438(15) 0.0457(15) 0.0060(13) 0.0190(12) 0.0046(12) C45 0.0229(12) 0.0333(13) 0.0252(12) 0.0090(10) 0.0084(10) 0.0092(10) C46 0.0350(14) 0.0341(14) 0.0335(13) 0.0017(11) 0.0183(11) 0.0119(12) C47 0.0371(14) 0.0259(12) 0.0260(12) 0.0044(10) 0.0117(11) 0.0094(11) C48 0.0582(19) 0.0315(15) 0.0564(18) -0.0041(14) 0.0255(16) 0.0091(14) _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 N1 1.9341(18) . ? Ru1 O3 2.0111(16) . ? Ru1 O2 2.0195(15) . ? Ru1 O1 2.0412(15) . ? Ru1 O5 2.0502(15) . ? Ru1 O4 2.0704(15) . ? Ru2 N2 1.9439(17) . ? Ru2 O6 2.0169(15) . ? Ru2 O9 2.0174(15) . ? Ru2 O10 2.0193(16) . ? Ru2 O8 2.0385(15) . ? Ru2 O7 2.0596(15) . ? O1 C14 1.287(3) . ? O2 C16 1.267(3) . ? O3 C18 1.283(3) . ? O4 C21 1.267(3) . ? O5 C23 1.285(3) . ? O6 C38 1.285(3) . ? O7 C40 1.265(3) . ? O8 C42 1.291(3) . ? O9 C45 1.267(3) . ? O10 C47 1.276(3) . ? N1 C1 1.332(3) . ? N1 H1 0.8800 . ? N2 C25 1.328(3) . ? N2 H2 0.8800 . ? C1 C14 1.433(3) . ? C1 C2 1.451(3) . ? C2 C3 1.401(3) . ? C2 C7 1.416(3) . ? C3 C4 1.378(3) . ? C3 H3 0.9500 . ? C4 C5 1.387(4) . ? C4 H4 0.9500 . ? C5 C6 1.373(4) . ? C5 H5 0.9500 . ? C6 C7 1.408(3) . ? C6 H6 0.9500 . ? C7 C8 1.471(3) . ? C8 C9 1.406(3) . ? C8 C13 1.413(3) . ? C9 C10 1.373(4) . ? C9 H9 0.9500 . ? C10 C11 1.387(4) . ? C10 H10 0.9500 . ? C11 C12 1.379(3) . ? C11 H11 0.9500 . ? C12 C13 1.404(3) . ? C12 H12 0.9500 . ? C13 C14 1.445(3) . ? C15 C16 1.508(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.403(3) . ? C17 C18 1.393(3) . ? C17 H17 0.9500 . ? C18 C19 1.509(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.506(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.401(3) . ? C22 C23 1.385(3) . ? C22 H22 0.9500 . ? C23 C24 1.507(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C38 1.428(3) . ? C25 C26 1.456(3) . ? C26 C27 1.407(3) . ? C26 C31 1.413(3) . ? C27 C28 1.375(3) . ? C27 H27 0.9500 . ? C28 C29 1.391(3) . ? C28 H28 0.9500 . ? C29 C30 1.379(3) . ? C29 H29 0.9500 . ? C30 C31 1.404(3) . ? C30 H30 0.9500 . ? C31 C32 1.474(3) . ? C32 C33 1.401(3) . ? C32 C37 1.410(3) . ? C33 C34 1.378(3) . ? C33 H33 0.9500 . ? C34 C35 1.397(3) . ? C34 H34 0.9500 . ? C35 C36 1.370(3) . ? C35 H35 0.9500 . ? C36 C37 1.404(3) . ? C36 H36 0.9500 . ? C37 C38 1.441(3) . ? C39 C40 1.515(3) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.399(4) . ? C41 C42 1.382(3) . ? C41 H41 0.9500 . ? C42 C43 1.512(3) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.506(3) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.409(3) . ? C46 C47 1.386(4) . ? C46 H46 0.9500 . ? C47 C48 1.515(4) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 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 N1 Ru1 O3 91.14(7) . . ? N1 Ru1 O2 95.17(7) . . ? O3 Ru1 O2 93.50(6) . . ? N1 Ru1 O1 78.89(7) . . ? O3 Ru1 O1 88.28(6) . . ? O2 Ru1 O1 173.84(6) . . ? N1 Ru1 O5 93.52(7) . . ? O3 Ru1 O5 175.29(6) . . ? O2 Ru1 O5 86.72(6) . . ? O1 Ru1 O5 91.99(6) . . ? N1 Ru1 O4 175.05(7) . . ? O3 Ru1 O4 85.71(6) . . ? O2 Ru1 O4 88.84(6) . . ? O1 Ru1 O4 97.17(6) . . ? O5 Ru1 O4 89.59(6) . . ? N2 Ru2 O6 79.36(7) . . ? N2 Ru2 O9 96.11(7) . . ? O6 Ru2 O9 174.25(6) . . ? N2 Ru2 O10 91.79(7) . . ? O6 Ru2 O10 90.61(6) . . ? O9 Ru2 O10 93.08(6) . . ? N2 Ru2 O8 91.42(6) . . ? O6 Ru2 O8 90.47(6) . . ? O9 Ru2 O8 86.08(6) . . ? O10 Ru2 O8 176.76(6) . . ? N2 Ru2 O7 174.91(7) . . ? O6 Ru2 O7 96.26(6) . . ? O9 Ru2 O7 88.41(6) . . ? O10 Ru2 O7 85.63(6) . . ? O8 Ru2 O7 91.21(6) . . ? C14 O1 Ru1 112.86(13) . . ? C16 O2 Ru1 122.29(15) . . ? C18 O3 Ru1 122.60(15) . . ? C21 O4 Ru1 126.04(15) . . ? C23 O5 Ru1 125.14(15) . . ? C38 O6 Ru2 113.62(13) . . ? C40 O7 Ru2 124.32(15) . . ? C42 O8 Ru2 123.52(15) . . ? C45 O9 Ru2 123.24(15) . . ? C47 O10 Ru2 122.49(15) . . ? C1 N1 Ru1 117.72(15) . . ? C1 N1 H1 121.1 . . ? Ru1 N1 H1 121.1 . . ? C25 N2 Ru2 116.99(14) . . ? C25 N2 H2 121.5 . . ? Ru2 N2 H2 121.5 . . ? N1 C1 C14 112.0(2) . . ? N1 C1 C2 127.3(2) . . ? C14 C1 C2 120.6(2) . . ? C3 C2 C7 119.2(2) . . ? C3 C2 C1 122.0(2) . . ? C7 C2 C1 118.8(2) . . ? C4 C3 C2 121.4(2) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.6(2) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 120.1(2) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 121.8(2) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C6 C7 C2 117.7(2) . . ? C6 C7 C8 122.3(2) . . ? C2 C7 C8 120.0(2) . . ? C9 C8 C13 117.2(2) . . ? C9 C8 C7 122.0(2) . . ? C13 C8 C7 120.8(2) . . ? C10 C9 C8 121.6(2) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 120.6(2) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 119.8(2) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 120.1(2) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C8 120.7(2) . . ? C12 C13 C14 120.5(2) . . ? C8 C13 C14 118.8(2) . . ? O1 C14 C1 117.4(2) . . ? O1 C14 C13 121.91(19) . . ? C1 C14 C13 120.5(2) . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C16 C17 125.6(2) . . ? O2 C16 C15 114.7(2) . . ? C17 C16 C15 119.6(2) . . ? C18 C17 C16 127.4(2) . . ? C18 C17 H17 116.3 . . ? C16 C17 H17 116.3 . . ? O3 C18 C17 125.8(2) . . ? O3 C18 C19 114.1(2) . . ? C17 C18 C19 120.1(2) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O4 C21 C22 125.0(2) . . ? O4 C21 C20 116.7(2) . . ? C22 C21 C20 118.2(2) . . ? C23 C22 C21 127.0(2) . . ? C23 C22 H22 116.5 . . ? C21 C22 H22 116.5 . . ? O5 C23 C22 126.2(2) . . ? O5 C23 C24 114.5(2) . . ? C22 C23 C24 119.2(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N2 C25 C38 112.64(19) . . ? N2 C25 C26 127.04(19) . . ? C38 C25 C26 120.32(19) . . ? C27 C26 C31 119.4(2) . . ? C27 C26 C25 121.8(2) . . ? C31 C26 C25 118.78(19) . . ? C28 C27 C26 120.8(2) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 120.3(2) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 119.6(2) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 121.8(2) . . ? C29 C30 H30 119.1 . . ? C31 C30 H30 119.1 . . ? C30 C31 C26 118.1(2) . . ? C30 C31 C32 121.5(2) . . ? C26 C31 C32 120.36(19) . . ? C33 C32 C37 116.9(2) . . ? C33 C32 C31 122.7(2) . . ? C37 C32 C31 120.4(2) . . ? C34 C33 C32 121.6(2) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C33 C34 C35 120.8(2) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C36 C35 C34 119.2(2) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C37 120.4(2) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C32 121.2(2) . . ? C36 C37 C38 119.7(2) . . ? C32 C37 C38 119.10(19) . . ? O6 C38 C25 117.3(2) . . ? O6 C38 C37 121.77(19) . . ? C25 C38 C37 120.89(19) . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O7 C40 C41 126.0(2) . . ? O7 C40 C39 115.7(2) . . ? C41 C40 C39 118.3(2) . . ? C42 C41 C40 127.0(2) . . ? C42 C41 H41 116.5 . . ? C40 C41 H41 116.5 . . ? O8 C42 C41 126.6(2) . . ? O8 C42 C43 114.1(2) . . ? C41 C42 C43 119.2(2) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 H44A 109.5 . . ? C45 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C45 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O9 C45 C46 125.3(2) . . ? O9 C45 C44 115.4(2) . . ? C46 C45 C44 119.3(2) . . ? C47 C46 C45 127.2(2) . . ? C47 C46 H46 116.4 . . ? C45 C46 H46 116.4 . . ? O10 C47 C46 126.7(2) . . ? O10 C47 C48 114.3(2) . . ? C46 C47 C48 119.0(2) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ru1 O1 C14 8.61(15) . . . . ? O3 Ru1 O1 C14 -82.90(15) . . . . ? O2 Ru1 O1 C14 24.0(7) . . . . ? O5 Ru1 O1 C14 101.81(15) . . . . ? O4 Ru1 O1 C14 -168.35(14) . . . . ? N1 Ru1 O2 C16 -74.13(17) . . . . ? O3 Ru1 O2 C16 17.34(17) . . . . ? O1 Ru1 O2 C16 -89.3(6) . . . . ? O5 Ru1 O2 C16 -167.38(17) . . . . ? O4 Ru1 O2 C16 102.96(17) . . . . ? N1 Ru1 O3 C18 84.63(17) . . . . ? O2 Ru1 O3 C18 -10.62(17) . . . . ? O1 Ru1 O3 C18 163.48(17) . . . . ? O5 Ru1 O3 C18 -103.1(8) . . . . ? O4 Ru1 O3 C18 -99.19(17) . . . . ? N1 Ru1 O4 C21 -137.2(7) . . . . ? O3 Ru1 O4 C21 172.22(18) . . . . ? O2 Ru1 O4 C21 78.62(18) . . . . ? O1 Ru1 O4 C21 -100.06(18) . . . . ? O5 Ru1 O4 C21 -8.11(18) . . . . ? N1 Ru1 O5 C23 -175.22(17) . . . . ? O3 Ru1 O5 C23 12.6(9) . . . . ? O2 Ru1 O5 C23 -80.24(17) . . . . ? O1 Ru1 O5 C23 105.79(17) . . . . ? O4 Ru1 O5 C23 8.63(17) . . . . ? N2 Ru2 O6 C38 2.33(14) . . . . ? O9 Ru2 O6 C38 40.6(7) . . . . ? O10 Ru2 O6 C38 -89.37(14) . . . . ? O8 Ru2 O6 C38 93.68(14) . . . . ? O7 Ru2 O6 C38 -175.04(14) . . . . ? N2 Ru2 O7 C40 -111.4(7) . . . . ? O6 Ru2 O7 C40 -80.86(18) . . . . ? O9 Ru2 O7 C40 95.79(18) . . . . ? O10 Ru2 O7 C40 -171.00(18) . . . . ? O8 Ru2 O7 C40 9.74(18) . . . . ? N2 Ru2 O8 C42 164.43(16) . . . . ? O6 Ru2 O8 C42 85.06(16) . . . . ? O9 Ru2 O8 C42 -99.54(16) . . . . ? O10 Ru2 O8 C42 -24.5(12) . . . . ? O7 Ru2 O8 C42 -11.22(16) . . . . ? N2 Ru2 O9 C45 -76.91(17) . . . . ? O6 Ru2 O9 C45 -114.7(6) . . . . ? O10 Ru2 O9 C45 15.23(17) . . . . ? O8 Ru2 O9 C45 -167.91(17) . . . . ? O7 Ru2 O9 C45 100.76(17) . . . . ? N2 Ru2 O10 C47 84.65(17) . . . . ? O6 Ru2 O10 C47 164.03(17) . . . . ? O9 Ru2 O10 C47 -11.57(17) . . . . ? O8 Ru2 O10 C47 -86.4(11) . . . . ? O7 Ru2 O10 C47 -99.74(17) . . . . ? O3 Ru1 N1 C1 78.83(16) . . . . ? O2 Ru1 N1 C1 172.44(15) . . . . ? O1 Ru1 N1 C1 -9.20(15) . . . . ? O5 Ru1 N1 C1 -100.54(16) . . . . ? O4 Ru1 N1 C1 28.4(9) . . . . ? O6 Ru2 N2 C25 -2.72(15) . . . . ? O9 Ru2 N2 C25 -179.14(15) . . . . ? O10 Ru2 N2 C25 87.57(15) . . . . ? O8 Ru2 N2 C25 -92.93(15) . . . . ? O7 Ru2 N2 C25 28.2(8) . . . . ? Ru1 N1 C1 C14 8.1(2) . . . . ? Ru1 N1 C1 C2 -174.02(16) . . . . ? N1 C1 C2 C3 0.6(3) . . . . ? C14 C1 C2 C3 178.3(2) . . . . ? N1 C1 C2 C7 179.4(2) . . . . ? C14 C1 C2 C7 -2.9(3) . . . . ? C7 C2 C3 C4 -3.9(3) . . . . ? C1 C2 C3 C4 174.9(2) . . . . ? C2 C3 C4 C5 -1.1(3) . . . . ? C3 C4 C5 C6 4.0(4) . . . . ? C4 C5 C6 C7 -2.0(4) . . . . ? C5 C6 C7 C2 -3.0(3) . . . . ? C5 C6 C7 C8 176.9(2) . . . . ? C3 C2 C7 C6 5.8(3) . . . . ? C1 C2 C7 C6 -173.0(2) . . . . ? C3 C2 C7 C8 -174.0(2) . . . . ? C1 C2 C7 C8 7.2(3) . . . . ? C6 C7 C8 C9 -7.5(3) . . . . ? C2 C7 C8 C9 172.3(2) . . . . ? C6 C7 C8 C13 174.0(2) . . . . ? C2 C7 C8 C13 -6.2(3) . . . . ? C13 C8 C9 C10 -0.6(3) . . . . ? C7 C8 C9 C10 -179.2(2) . . . . ? C8 C9 C10 C11 0.7(4) . . . . ? C9 C10 C11 C12 -0.5(4) . . . . ? C10 C11 C12 C13 0.3(4) . . . . ? C11 C12 C13 C8 -0.3(3) . . . . ? C11 C12 C13 C14 178.0(2) . . . . ? C9 C8 C13 C12 0.5(3) . . . . ? C7 C8 C13 C12 179.1(2) . . . . ? C9 C8 C13 C14 -177.9(2) . . . . ? C7 C8 C13 C14 0.7(3) . . . . ? Ru1 O1 C14 C1 -7.0(2) . . . . ? Ru1 O1 C14 C13 177.31(16) . . . . ? N1 C1 C14 O1 -0.3(3) . . . . ? C2 C1 C14 O1 -178.29(19) . . . . ? N1 C1 C14 C13 175.49(19) . . . . ? C2 C1 C14 C13 -2.5(3) . . . . ? C12 C13 C14 O1 0.8(3) . . . . ? C8 C13 C14 O1 179.1(2) . . . . ? C12 C13 C14 C1 -174.8(2) . . . . ? C8 C13 C14 C1 3.6(3) . . . . ? Ru1 O2 C16 C17 -14.2(3) . . . . ? Ru1 O2 C16 C15 167.43(17) . . . . ? O2 C16 C17 C18 -1.4(4) . . . . ? C15 C16 C17 C18 176.9(2) . . . . ? Ru1 O3 C18 C17 0.2(3) . . . . ? Ru1 O3 C18 C19 178.79(14) . . . . ? C16 C17 C18 O3 9.5(4) . . . . ? C16 C17 C18 C19 -169.0(2) . . . . ? Ru1 O4 C21 C22 2.3(3) . . . . ? Ru1 O4 C21 C20 178.78(15) . . . . ? O4 C21 C22 C23 7.2(4) . . . . ? C20 C21 C22 C23 -169.3(2) . . . . ? Ru1 O5 C23 C22 -3.6(3) . . . . ? Ru1 O5 C23 C24 -179.80(15) . . . . ? C21 C22 C23 O5 -6.5(4) . . . . ? C21 C22 C23 C24 169.6(2) . . . . ? Ru2 N2 C25 C38 2.6(2) . . . . ? Ru2 N2 C25 C26 -177.40(16) . . . . ? N2 C25 C26 C27 4.7(3) . . . . ? C38 C25 C26 C27 -175.35(19) . . . . ? N2 C25 C26 C31 -176.9(2) . . . . ? C38 C25 C26 C31 3.1(3) . . . . ? C31 C26 C27 C28 -0.8(3) . . . . ? C25 C26 C27 C28 177.59(19) . . . . ? C26 C27 C28 C29 0.4(3) . . . . ? C27 C28 C29 C30 0.0(3) . . . . ? C28 C29 C30 C31 0.0(3) . . . . ? C29 C30 C31 C26 -0.4(3) . . . . ? C29 C30 C31 C32 -177.8(2) . . . . ? C27 C26 C31 C30 0.8(3) . . . . ? C25 C26 C31 C30 -177.63(19) . . . . ? C27 C26 C31 C32 178.22(19) . . . . ? C25 C26 C31 C32 -0.2(3) . . . . ? C30 C31 C32 C33 -3.0(3) . . . . ? C26 C31 C32 C33 179.7(2) . . . . ? C30 C31 C32 C37 174.33(19) . . . . ? C26 C31 C32 C37 -3.0(3) . . . . ? C37 C32 C33 C34 -1.8(3) . . . . ? C31 C32 C33 C34 175.6(2) . . . . ? C32 C33 C34 C35 0.8(4) . . . . ? C33 C34 C35 C36 0.2(4) . . . . ? C34 C35 C36 C37 -0.1(3) . . . . ? C35 C36 C37 C32 -1.0(3) . . . . ? C35 C36 C37 C38 -179.9(2) . . . . ? C33 C32 C37 C36 1.9(3) . . . . ? C31 C32 C37 C36 -175.61(19) . . . . ? C33 C32 C37 C38 -179.2(2) . . . . ? C31 C32 C37 C38 3.3(3) . . . . ? Ru2 O6 C38 C25 -1.7(2) . . . . ? Ru2 O6 C38 C37 -179.39(15) . . . . ? N2 C25 C38 O6 -0.5(3) . . . . ? C26 C25 C38 O6 179.47(18) . . . . ? N2 C25 C38 C37 177.21(18) . . . . ? C26 C25 C38 C37 -2.8(3) . . . . ? C36 C37 C38 O6 -3.9(3) . . . . ? C32 C37 C38 O6 177.21(19) . . . . ? C36 C37 C38 C25 178.48(19) . . . . ? C32 C37 C38 C25 -0.4(3) . . . . ? Ru2 O7 C40 C41 -3.3(3) . . . . ? Ru2 O7 C40 C39 178.81(15) . . . . ? O7 C40 C41 C42 -6.4(4) . . . . ? C39 C40 C41 C42 171.5(2) . . . . ? Ru2 O8 C42 C41 6.6(3) . . . . ? Ru2 O8 C42 C43 -175.06(15) . . . . ? C40 C41 C42 O8 4.5(4) . . . . ? C40 C41 C42 C43 -173.7(2) . . . . ? Ru2 O9 C45 C46 -11.6(3) . . . . ? Ru2 O9 C45 C44 169.88(15) . . . . ? O9 C45 C46 C47 -1.0(4) . . . . ? C44 C45 C46 C47 177.5(2) . . . . ? Ru2 O10 C47 C46 4.2(3) . . . . ? Ru2 O10 C47 C48 -175.78(16) . . . . ? C45 C46 C47 O10 5.2(4) . . . . ? C45 C46 C47 C48 -174.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.327 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.056 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 121 9 ' ' 2 0.000 0.500 0.000 121 9 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 963960'