# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email xray@chem.iitb.ac.in _publ_contact_author_name 'Mobin Shaikh' _publ_author_name G.Lahiri data_gkl223 _database_code_depnum_ccdc_archive 'CCDC 827492' #TrackingRef 'gkl223.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H14 N4 O5' _chemical_formula_weight 282.26 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.6996(5) _cell_length_b 16.5546(8) _cell_length_c 11.5646(11) _cell_angle_alpha 90.00 _cell_angle_beta 106.310(8) _cell_angle_gamma 90.00 _cell_volume 1231.00(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2531 _cell_measurement_theta_min 3.3939 _cell_measurement_theta_max 32.5131 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.122 _exptl_absorpt_correction_T_min 0.9724 _exptl_absorpt_correction_T_max 0.9891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) 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 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _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 8437 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2148 _reflns_number_gt 1412 _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^)+(0.0282P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2148 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0656 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 0.830 _refine_ls_restrained_S_all 0.830 _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 O1 O 0.11663(19) 0.00179(7) 0.72946(11) 0.0265(3) Uani 1 1 d . . . O2 O 0.05144(19) 0.12874(7) 0.66235(11) 0.0276(3) Uani 1 1 d . . . N1 N 0.1947(2) 0.18942(8) 0.89323(13) 0.0179(4) Uani 1 1 d . . . H1 H 0.1655 0.2281 0.8389 0.021 Uiso 1 1 calc R . . N2 N 0.2896(2) 0.13111(8) 1.07270(13) 0.0184(4) Uani 1 1 d . . . N3 N 0.2279(2) -0.07349(8) 0.94107(13) 0.0178(4) Uani 1 1 d . . . H3 H 0.1946 -0.0701 0.8620 0.021 Uiso 1 1 calc R . . N4 N 0.3059(2) -0.03832(8) 1.13015(13) 0.0181(4) Uani 1 1 d . . . H4 H 0.3321 -0.0081 1.1953 0.022 Uiso 1 1 calc R . . C1 C 0.1114(3) 0.07770(11) 0.74404(16) 0.0200(4) Uani 1 1 d . . . C2 C 0.1813(2) 0.10859(10) 0.87007(16) 0.0159(4) Uani 1 1 d . . . C3 C 0.2600(2) 0.19996(10) 1.01294(16) 0.0195(4) Uani 1 1 d . . . H3A H 0.2825 0.2515 1.0506 0.023 Uiso 1 1 calc R . . C4 C 0.2411(2) 0.07298(10) 0.98312(15) 0.0152(4) Uani 1 1 d . . . C5 C 0.2567(2) -0.01118(10) 1.01693(16) 0.0166(4) Uani 1 1 d . . . C6 C 0.3086(2) -0.12239(9) 1.12778(16) 0.0169(4) Uani 1 1 d . . . C7 C 0.3486(3) -0.17886(10) 1.22033(16) 0.0213(4) Uani 1 1 d . . . H7 H 0.3830 -0.1632 1.3026 0.026 Uiso 1 1 calc R . . C8 C 0.3355(2) -0.25904(11) 1.18613(17) 0.0236(5) Uani 1 1 d . . . H8 H 0.3590 -0.2998 1.2463 0.028 Uiso 1 1 calc R . . C9 C 0.2885(3) -0.28172(11) 1.06489(17) 0.0234(5) Uani 1 1 d . . . H9 H 0.2828 -0.3375 1.0452 0.028 Uiso 1 1 calc R . . C10 C 0.2501(2) -0.22563(10) 0.97307(16) 0.0205(4) Uani 1 1 d . . . H10 H 0.2192 -0.2412 0.8909 0.025 Uiso 1 1 calc R . . C11 C 0.2594(2) -0.14493(10) 1.00775(16) 0.0166(4) Uani 1 1 d . . . O111 O 0.3691(3) 0.02833(9) 0.35301(13) 0.0335(4) Uani 1 1 d . . . O222 O 0.6473(2) 0.16729(7) 0.26853(13) 0.0241(3) Uani 1 1 d . . . O333 O 0.7903(2) 0.05828(8) 0.46772(13) 0.0272(4) Uani 1 1 d . . . H555 H 0.686(3) 0.1344(13) 0.330(2) 0.062(8) Uiso 1 1 d . . . H666 H 0.518(4) 0.1504(13) 0.213(2) 0.077(8) Uiso 1 1 d . . . H444 H 0.852(3) 0.0334(14) 0.416(2) 0.073(9) Uiso 1 1 d . . . H222 H 0.498(4) 0.0354(15) 0.399(2) 0.081(10) Uiso 1 1 d . . . H333 H 0.889(3) 0.0835(14) 0.530(2) 0.071(8) Uiso 1 1 d . . . H111 H 0.301(4) 0.0079(17) 0.396(3) 0.100(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0410(8) 0.0177(8) 0.0193(8) -0.0019(6) 0.0060(6) 0.0015(6) O2 0.0407(8) 0.0213(7) 0.0164(8) 0.0026(6) 0.0011(6) 0.0000(6) N1 0.0212(8) 0.0158(8) 0.0161(9) 0.0027(6) 0.0041(7) 0.0015(6) N2 0.0196(8) 0.0177(8) 0.0174(9) -0.0009(7) 0.0046(7) 0.0000(6) N3 0.0206(8) 0.0183(8) 0.0139(9) 0.0004(7) 0.0038(6) 0.0005(6) N4 0.0206(8) 0.0184(8) 0.0146(9) -0.0014(7) 0.0037(7) 0.0001(6) C1 0.0180(10) 0.0210(11) 0.0210(11) -0.0004(9) 0.0055(8) -0.0008(8) C2 0.0133(9) 0.0159(9) 0.0182(10) -0.0011(8) 0.0038(8) -0.0010(7) C3 0.0176(10) 0.0206(11) 0.0193(11) -0.0038(8) 0.0036(8) 0.0000(8) C4 0.0115(9) 0.0167(10) 0.0168(11) -0.0006(8) 0.0030(8) 0.0001(7) C5 0.0118(10) 0.0192(10) 0.0182(11) 0.0008(8) 0.0032(8) -0.0015(7) C6 0.0139(10) 0.0150(10) 0.0215(11) 0.0008(8) 0.0044(8) 0.0005(8) C7 0.0215(10) 0.0237(11) 0.0188(11) 0.0043(8) 0.0059(8) 0.0017(8) C8 0.0218(11) 0.0251(12) 0.0248(12) 0.0083(9) 0.0080(9) 0.0010(8) C9 0.0206(11) 0.0171(10) 0.0341(13) 0.0004(9) 0.0103(9) -0.0001(8) C10 0.0197(10) 0.0188(10) 0.0230(11) 0.0000(8) 0.0058(8) -0.0025(8) C11 0.0130(9) 0.0174(10) 0.0199(11) 0.0034(8) 0.0054(8) 0.0019(7) O111 0.0350(10) 0.0433(9) 0.0218(9) -0.0038(7) 0.0072(8) -0.0117(7) O222 0.0302(8) 0.0201(8) 0.0182(8) 0.0005(6) 0.0004(6) -0.0008(6) O333 0.0276(8) 0.0319(8) 0.0206(8) -0.0035(6) 0.0043(7) 0.0008(6) _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 O1 C1 1.270(2) . ? O2 C1 1.247(2) . ? N1 C3 1.341(2) . ? N1 C2 1.363(2) . ? N1 H1 0.8800 . ? N2 C3 1.319(2) . ? N2 C4 1.384(2) . ? N3 C5 1.333(2) . ? N3 C11 1.395(2) . ? N3 H3 0.8800 . ? N4 C5 1.335(2) . ? N4 C6 1.392(2) . ? N4 H4 0.8800 . ? C1 C2 1.491(2) . ? C2 C4 1.387(2) . ? C3 H3A 0.9500 . ? C4 C5 1.443(2) . ? C6 C11 1.385(2) . ? C6 C7 1.389(2) . ? C7 C8 1.381(2) . ? C7 H7 0.9500 . ? C8 C9 1.399(2) . ? C8 H8 0.9500 . ? C9 C10 1.379(2) . ? C9 H9 0.9500 . ? C10 C11 1.391(2) . ? C10 H10 0.9500 . ? O111 H222 0.88(3) . ? O111 H111 0.84(3) . ? O222 H555 0.87(2) . ? O222 H666 0.97(2) . ? O333 H444 0.92(3) . ? O333 H333 0.93(2) . ? 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 C3 N1 C2 108.36(14) . . ? C3 N1 H1 125.8 . . ? C2 N1 H1 125.8 . . ? C3 N2 C4 103.86(15) . . ? C5 N3 C11 108.71(14) . . ? C5 N3 H3 125.6 . . ? C11 N3 H3 125.6 . . ? C5 N4 C6 108.55(15) . . ? C5 N4 H4 125.7 . . ? C6 N4 H4 125.7 . . ? O2 C1 O1 125.81(17) . . ? O2 C1 C2 117.02(16) . . ? O1 C1 C2 117.17(15) . . ? N1 C2 C4 104.27(15) . . ? N1 C2 C1 120.95(15) . . ? C4 C2 C1 134.77(15) . . ? N2 C3 N1 112.71(15) . . ? N2 C3 H3A 123.6 . . ? N1 C3 H3A 123.6 . . ? N2 C4 C2 110.79(15) . . ? N2 C4 C5 118.99(15) . . ? C2 C4 C5 130.22(16) . . ? N3 C5 N4 109.60(15) . . ? N3 C5 C4 125.66(16) . . ? N4 C5 C4 124.74(16) . . ? C11 C6 C7 122.08(15) . . ? C11 C6 N4 106.76(15) . . ? C7 C6 N4 131.16(17) . . ? C8 C7 C6 116.30(17) . . ? C8 C7 H7 121.8 . . ? C6 C7 H7 121.8 . . ? C7 C8 C9 121.56(17) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C10 C9 C8 122.11(17) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 C10 C11 116.16(17) . . ? C9 C10 H10 121.9 . . ? C11 C10 H10 121.9 . . ? C6 C11 C10 121.77(16) . . ? C6 C11 N3 106.39(14) . . ? C10 C11 N3 131.84(17) . . ? H222 O111 H111 107(2) . . ? H555 O222 H666 111.6(19) . . ? H444 O333 H333 110.4(19) . . ? 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 C3 N1 C2 C4 0.40(18) . . . . ? C3 N1 C2 C1 179.73(15) . . . . ? O2 C1 C2 N1 -5.3(2) . . . . ? O1 C1 C2 N1 175.30(15) . . . . ? O2 C1 C2 C4 173.82(18) . . . . ? O1 C1 C2 C4 -5.6(3) . . . . ? C4 N2 C3 N1 0.70(19) . . . . ? C2 N1 C3 N2 -0.7(2) . . . . ? C3 N2 C4 C2 -0.43(19) . . . . ? C3 N2 C4 C5 179.99(14) . . . . ? N1 C2 C4 N2 0.02(19) . . . . ? C1 C2 C4 N2 -179.17(17) . . . . ? N1 C2 C4 C5 179.54(16) . . . . ? C1 C2 C4 C5 0.3(3) . . . . ? C11 N3 C5 N4 0.07(18) . . . . ? C11 N3 C5 C4 179.12(16) . . . . ? C6 N4 C5 N3 -0.16(19) . . . . ? C6 N4 C5 C4 -179.21(14) . . . . ? N2 C4 C5 N3 -175.54(16) . . . . ? C2 C4 C5 N3 5.0(3) . . . . ? N2 C4 C5 N4 3.4(2) . . . . ? C2 C4 C5 N4 -176.12(17) . . . . ? C5 N4 C6 C11 0.18(19) . . . . ? C5 N4 C6 C7 -179.38(18) . . . . ? C11 C6 C7 C8 -0.3(3) . . . . ? N4 C6 C7 C8 179.17(16) . . . . ? C6 C7 C8 C9 1.2(3) . . . . ? C7 C8 C9 C10 -0.8(3) . . . . ? C8 C9 C10 C11 -0.4(3) . . . . ? C7 C6 C11 C10 -0.9(3) . . . . ? N4 C6 C11 C10 179.46(15) . . . . ? C7 C6 C11 N3 179.48(15) . . . . ? N4 C6 C11 N3 -0.14(18) . . . . ? C9 C10 C11 C6 1.3(2) . . . . ? C9 C10 C11 N3 -179.23(17) . . . . ? C5 N3 C11 C6 0.04(18) . . . . ? C5 N3 C11 C10 -179.50(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.157 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.047 # Attachment '[1](ClO4).cif' ##Title:Selective recognition of fluoride and acetate ##by the newly designed ruthenium framework. ##Experimental and theoretical investigations ##Communicated to Dalton Trans. ##By Tanaya Kundu, Abhishek Dutta Chowdhury, Dipanwita De, ##Shaikh M Mobin, Vedavati G. Puranik, Anindya Datta and Goutam Kumar Lahiri ##Department of Chemistry, Indian Institute of Technology Bombay, Powai, Mumbai-400076, India. ##and Centre For Materials Characterisation ##National Chemical Laboratory,Dr. Homi Bhabha Road, Pune 411 008, India. data_[1](ClO4) _database_code_depnum_ccdc_archive 'CCDC 827493' #TrackingRef '[1](ClO4).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common rutheniumcomplexes _chemical_melting_point ? _chemical_formula_moiety C31H23N8O6ClRu.ClO4.2H2O _chemical_formula_sum 'C31 H27 Cl N8 O8 Ru' _chemical_formula_weight 776.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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 19.8792(7) _cell_length_b 20.3466(5) _cell_length_c 18.3949(6) _cell_angle_alpha 90.00 _cell_angle_beta 117.034(4) _cell_angle_gamma 90.00 _cell_volume 6627.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7174 _cell_measurement_theta_min 3.3266 _cell_measurement_theta_max 29.2384 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3152 _exptl_absorpt_coefficient_mu 0.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8224 _exptl_absorpt_correction_T_max 0.8712 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _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 24219 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5819 _reflns_number_gt 3073 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL and PLATON' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0931P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5819 _refine_ls_number_parameters 472 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1530 _refine_ls_wR_factor_gt 0.1381 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.884 _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 Ru Ru 0.81355(3) -0.05107(2) 0.90611(2) 0.0815(2) Uani 1 1 d . . . N1 N 0.7501(3) 0.0282(2) 0.9064(3) 0.0853(13) Uani 1 1 d . . . N2 N 0.6755(3) 0.1074(3) 0.9047(3) 0.0900(13) Uani 1 1 d . . . H2 H 0.6355 0.1329 0.8869 0.12(2) Uiso 1 1 calc R . . N3 N 0.8070(2) 0.1693(2) 1.1063(3) 0.0851(12) Uani 1 1 d . . . H3 H 0.8481 0.1452 1.1224 0.102 Uiso 1 1 calc R . . N4 N 0.6902(3) 0.2063(3) 1.0254(3) 0.0962(14) Uani 1 1 d . . . N5 N 0.7759(3) -0.1103(3) 0.9709(3) 0.0936(15) Uani 1 1 d . . . N6 N 0.8853(3) -0.1286(2) 0.9331(2) 0.0790(12) Uani 1 1 d . . . N7 N 0.8558(2) 0.00286(19) 0.8426(2) 0.0747(11) Uani 1 1 d . . . N8 N 0.7439(2) -0.0792(2) 0.7895(2) 0.0806(12) Uani 1 1 d . . . O1 O 0.8857(2) -0.0100(2) 1.0201(2) 0.0933(11) Uani 1 1 d . . . O2 O 0.8979(2) 0.07287(19) 1.1049(2) 0.0966(12) Uani 1 1 d . . . C1 C 0.8615(4) 0.0409(4) 1.0391(4) 0.0883(17) Uani 1 1 d . . . C2 C 0.7864(3) 0.0634(3) 0.9810(3) 0.0738(14) Uani 1 1 d . . . C3 C 0.6874(4) 0.0539(4) 0.8643(3) 0.0959(18) Uani 1 1 d . . . H3A H 0.6522 0.0391 0.8116 0.115 Uiso 1 1 calc R . . C4 C 0.7373(4) 0.1117(3) 0.9757(3) 0.0884(16) Uani 1 1 d . . . C5 C 0.7437(3) 0.1646(3) 1.0357(3) 0.0867(16) Uani 1 1 d . . . C6 C 0.7210(4) 0.2423(3) 1.0973(3) 0.0882(16) Uani 1 1 d . . . C7 C 0.6903(4) 0.2949(3) 1.1222(4) 0.0995(18) Uani 1 1 d . . . H7 H 0.6413 0.3115 1.0877 0.119 Uiso 1 1 calc R . . C8 C 0.7339(5) 0.3217(3) 1.1985(4) 0.113(2) Uani 1 1 d . . . H8 H 0.7139 0.3563 1.2174 0.135 Uiso 1 1 calc R . . C9 C 0.8068(5) 0.2989(4) 1.2483(4) 0.117(2) Uani 1 1 d . . . H9 H 0.8360 0.3190 1.2999 0.141 Uiso 1 1 calc R . . C10 C 0.8368(4) 0.2481(4) 1.2241(4) 0.114(2) Uani 1 1 d . . . H10 H 0.8862 0.2322 1.2583 0.137 Uiso 1 1 calc R . . C11 C 0.7938(4) 0.2208(3) 1.1491(4) 0.0926(17) Uani 1 1 d . . . C12 C 0.7158(5) -0.0987(4) 0.9841(4) 0.118(2) Uani 1 1 d . . . H12 H 0.6818 -0.0645 0.9546 0.141 Uiso 1 1 calc R . . C13 C 0.7019(6) -0.1356(5) 1.0400(5) 0.135(3) Uani 1 1 d . . . H13 H 0.6589 -0.1271 1.0484 0.162 Uiso 1 1 calc R . . C14 C 0.7510(7) -0.1832(5) 1.0814(5) 0.143(4) Uani 1 1 d . . . H14 H 0.7431 -0.2078 1.1207 0.171 Uiso 1 1 calc R . . C15 C 0.8133(5) -0.1979(3) 1.0687(4) 0.121(3) Uani 1 1 d . . . H15 H 0.8476 -0.2317 1.0990 0.145 Uiso 1 1 calc R . . C16 C 0.8236(4) -0.1616(3) 1.0104(3) 0.0963(19) Uani 1 1 d . . . C17 C 0.8826(4) -0.1733(3) 0.9867(3) 0.0874(17) Uani 1 1 d . . . C18 C 0.9329(5) -0.2260(3) 1.0139(4) 0.108(2) Uani 1 1 d . . . H18 H 0.9308 -0.2566 1.0519 0.130 Uiso 1 1 calc R . . C19 C 0.9843(4) -0.2335(3) 0.9861(4) 0.118(2) Uani 1 1 d . . . H19 H 1.0186 -0.2694 1.0040 0.141 Uiso 1 1 calc R . . C20 C 0.9868(4) -0.1888(4) 0.9316(4) 0.111(2) Uani 1 1 d . . . H20 H 1.0223 -0.1936 0.9107 0.133 Uiso 1 1 calc R . . C21 C 0.9370(4) -0.1368(3) 0.9075(3) 0.0951(18) Uani 1 1 d . . . H21 H 0.9400 -0.1054 0.8709 0.114 Uiso 1 1 calc R . . C22 C 0.9177(3) 0.0412(3) 0.8768(4) 0.0928(17) Uani 1 1 d . . . H22 H 0.9459 0.0429 0.9345 0.111 Uiso 1 1 calc R . . C23 C 0.9410(4) 0.0783(3) 0.8290(4) 0.107(2) Uani 1 1 d . . . H23 H 0.9834 0.1065 0.8541 0.128 Uiso 1 1 calc R . . C24 C 0.9027(4) 0.0741(3) 0.7454(4) 0.1009(19) Uani 1 1 d . . . H24 H 0.9188 0.0984 0.7120 0.121 Uiso 1 1 calc R . . C25 C 0.8415(4) 0.0344(3) 0.7120(4) 0.0874(16) Uani 1 1 d . . . H25 H 0.8142 0.0310 0.6543 0.105 Uiso 1 1 calc R . . C26 C 0.8176(3) -0.0015(3) 0.7602(3) 0.0749(14) Uani 1 1 d . . . C27 C 0.7530(3) -0.0465(3) 0.7308(3) 0.0765(14) Uani 1 1 d . . . C28 C 0.7036(4) -0.0553(3) 0.6492(3) 0.0944(17) Uani 1 1 d . . . H28 H 0.7094 -0.0304 0.6087 0.113 Uiso 1 1 calc R . . C29 C 0.6468(4) -0.0998(4) 0.6272(4) 0.111(2) Uani 1 1 d . . . H29 H 0.6130 -0.1065 0.5712 0.134 Uiso 1 1 calc R . . C30 C 0.6386(3) -0.1343(4) 0.6851(4) 0.111(2) Uani 1 1 d . . . H30 H 0.5993 -0.1660 0.6703 0.133 Uiso 1 1 calc R . . C31 C 0.6880(3) -0.1233(3) 0.7669(4) 0.0992(18) Uani 1 1 d . . . H31 H 0.6820 -0.1476 0.8076 0.119 Uiso 1 1 calc R . . Cl1 Cl 0.5246(5) 0.0549(6) 0.5908(6) 0.254(4) Uani 0.50 1 d PD . . O3 O 0.5252(8) 0.1146(5) 0.5657(8) 0.194(6) Uani 0.50 1 d PD . . O4 O 0.5679(13) 0.0402(8) 0.6694(8) 0.301(13) Uani 0.50 1 d PD . . O5 O 0.4540(13) 0.0244(17) 0.5726(18) 0.50(3) Uani 0.50 1 d PD . . O6 O 0.5489(15) 0.0270(15) 0.5378(15) 0.58(5) Uani 0.50 1 d PD . . Cl2 Cl 0.5000 0.22663(12) 0.2500 0.1089(7) Uani 1 2 d S . . O7 O 0.4572(4) 0.2650(3) 0.2742(4) 0.221(3) Uani 1 1 d . . . O8 O 0.4536(3) 0.1861(2) 0.1846(3) 0.1424(18) Uani 1 1 d . . . O9 O 0.5000 0.9577(6) 0.7500 0.234(11) Uani 0.50 2 d SP A 1 O10 O 0.5000 0.3909(4) 0.7500 0.211(5) Uani 1 2 d S B 2 O11 O 0.5460(4) 0.1795(4) 0.8573(6) 0.259(4) Uani 1 1 d . C 3 O12 O 0.5000 0.2796(7) 0.7500 0.140(5) Uani 0.50 2 d SP D 4 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 Ru 0.0864(4) 0.0972(4) 0.0579(3) -0.0058(2) 0.0302(2) -0.0286(2) N1 0.075(3) 0.110(3) 0.064(3) -0.002(3) 0.025(3) -0.021(3) N2 0.066(3) 0.122(4) 0.066(3) 0.000(3) 0.016(3) -0.012(3) N3 0.085(3) 0.105(3) 0.061(3) -0.004(2) 0.030(3) -0.017(3) N4 0.092(4) 0.125(4) 0.070(3) -0.008(3) 0.036(3) -0.022(3) N5 0.106(4) 0.109(4) 0.074(3) -0.027(3) 0.048(3) -0.051(3) N6 0.087(3) 0.085(3) 0.060(2) 0.003(2) 0.029(2) -0.022(2) N7 0.072(3) 0.083(3) 0.065(3) 0.006(2) 0.027(2) -0.008(2) N8 0.077(3) 0.099(3) 0.067(3) -0.018(2) 0.034(2) -0.019(2) O1 0.095(3) 0.103(3) 0.068(2) 0.001(2) 0.026(2) -0.020(2) O2 0.092(3) 0.121(3) 0.056(2) -0.014(2) 0.0147(19) -0.019(2) C1 0.092(5) 0.104(5) 0.074(4) 0.015(4) 0.042(4) -0.023(4) C2 0.063(3) 0.094(4) 0.060(3) 0.003(3) 0.024(3) -0.016(3) C3 0.078(4) 0.135(5) 0.055(3) -0.011(4) 0.014(3) -0.029(4) C4 0.084(4) 0.118(5) 0.063(3) 0.008(3) 0.033(3) -0.017(4) C5 0.073(4) 0.113(5) 0.075(4) 0.011(4) 0.035(3) -0.007(3) C6 0.097(5) 0.104(4) 0.068(4) -0.004(3) 0.042(4) -0.019(4) C7 0.094(4) 0.112(5) 0.103(5) 0.010(4) 0.054(4) -0.005(4) C8 0.142(7) 0.119(5) 0.095(5) -0.011(4) 0.070(5) -0.005(5) C9 0.139(7) 0.138(6) 0.070(4) -0.017(4) 0.043(5) -0.030(5) C10 0.119(5) 0.138(6) 0.077(4) 0.003(4) 0.037(4) -0.016(5) C11 0.106(5) 0.107(5) 0.071(4) -0.001(4) 0.046(4) -0.023(4) C12 0.140(6) 0.134(6) 0.098(5) -0.039(4) 0.070(5) -0.069(5) C13 0.193(9) 0.136(7) 0.110(6) -0.042(5) 0.099(6) -0.083(7) C14 0.230(11) 0.137(7) 0.099(6) -0.045(5) 0.107(7) -0.101(7) C15 0.175(7) 0.122(5) 0.069(4) -0.016(4) 0.058(4) -0.072(5) C16 0.123(5) 0.096(5) 0.063(3) -0.019(3) 0.036(4) -0.051(4) C17 0.106(5) 0.089(4) 0.056(3) -0.004(3) 0.027(3) -0.042(4) C18 0.130(6) 0.093(5) 0.078(4) 0.016(3) 0.026(4) -0.035(5) C19 0.118(6) 0.104(5) 0.100(5) 0.023(4) 0.022(4) -0.018(4) C20 0.117(5) 0.114(5) 0.091(4) 0.003(4) 0.038(4) -0.013(4) C21 0.099(5) 0.099(5) 0.075(4) 0.015(3) 0.028(4) -0.014(4) C22 0.085(4) 0.104(4) 0.083(4) 0.004(3) 0.033(3) -0.024(3) C23 0.101(5) 0.109(5) 0.111(5) 0.026(4) 0.049(4) -0.018(4) C24 0.101(5) 0.110(5) 0.112(5) 0.035(4) 0.067(4) 0.009(4) C25 0.095(5) 0.102(4) 0.075(4) 0.016(3) 0.047(3) 0.023(4) C26 0.073(4) 0.090(4) 0.064(3) 0.011(3) 0.032(3) 0.014(3) C27 0.081(4) 0.093(4) 0.059(3) -0.008(3) 0.035(3) 0.006(3) C28 0.085(4) 0.127(5) 0.063(3) -0.011(3) 0.026(3) 0.014(4) C29 0.092(5) 0.164(7) 0.070(4) -0.034(4) 0.029(4) 0.003(5) C30 0.082(4) 0.139(6) 0.106(5) -0.057(5) 0.038(4) -0.028(4) C31 0.089(4) 0.122(5) 0.087(4) -0.032(4) 0.040(4) -0.030(4) Cl1 0.165(8) 0.299(10) 0.253(9) 0.103(8) 0.057(7) 0.112(7) O3 0.229(15) 0.107(8) 0.186(12) 0.048(8) 0.042(10) 0.014(8) O4 0.35(3) 0.199(14) 0.153(12) 0.014(10) -0.056(15) 0.038(14) O5 0.27(3) 0.96(10) 0.39(4) 0.16(5) 0.25(3) 0.17(4) O6 0.22(3) 0.55(7) 0.88(13) 0.42(9) 0.16(6) 0.18(4) Cl2 0.146(2) 0.0821(15) 0.0995(16) 0.000 0.0566(16) 0.000 O7 0.284(8) 0.166(5) 0.219(7) -0.007(5) 0.121(6) 0.113(6) O8 0.186(5) 0.125(4) 0.109(3) -0.014(3) 0.059(3) -0.039(3) O9 0.34(3) 0.049(7) 0.44(3) 0.000 0.29(3) 0.000 O10 0.247(10) 0.176(7) 0.067(4) 0.000 -0.053(5) 0.000 O11 0.229(7) 0.244(7) 0.397(11) 0.124(7) 0.224(8) 0.142(6) O12 0.131(11) 0.150(11) 0.157(12) 0.000 0.082(10) 0.000 _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 Ru N6 2.031(5) . ? Ru N8 2.037(4) . ? Ru N7 2.041(4) . ? Ru N1 2.049(5) . ? Ru N5 2.060(5) . ? Ru O1 2.102(4) . ? N1 C3 1.245(7) . ? N1 C2 1.420(6) . ? N2 C4 1.327(7) . ? N2 C3 1.398(7) . ? N2 H2 0.8800 . ? N3 C5 1.340(6) . ? N3 C11 1.406(7) . ? N3 H3 0.8800 . ? N4 C5 1.307(7) . ? N4 C6 1.387(7) . ? N5 C12 1.343(8) . ? N5 C16 1.375(8) . ? N6 C21 1.322(7) . ? N6 C17 1.361(6) . ? N7 C22 1.347(6) . ? N7 C26 1.356(6) . ? N8 C31 1.337(7) . ? N8 C27 1.349(6) . ? O1 C1 1.256(7) . ? O2 C1 1.271(7) . ? C1 C2 1.460(8) . ? C2 C4 1.358(7) . ? C3 H3A 0.9500 . ? C4 C5 1.503(8) . ? C6 C11 1.394(8) . ? C6 C7 1.407(8) . ? C7 C8 1.384(9) . ? C7 H7 0.9500 . ? C8 C9 1.396(9) . ? C8 H8 0.9500 . ? C9 C10 1.366(9) . ? C9 H9 0.9500 . ? C10 C11 1.367(8) . ? C10 H10 0.9500 . ? C12 C13 1.399(10) . ? C12 H12 0.9500 . ? C13 C14 1.340(11) . ? C13 H13 0.9500 . ? C14 C15 1.391(11) . ? C14 H14 0.9500 . ? C15 C16 1.393(8) . ? C15 H15 0.9500 . ? C16 C17 1.444(9) . ? C17 C18 1.395(9) . ? C18 C19 1.343(9) . ? C18 H18 0.9500 . ? C19 C20 1.371(9) . ? C19 H19 0.9500 . ? C20 C21 1.376(8) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.386(8) . ? C22 H22 0.9500 . ? C23 C24 1.373(8) . ? C23 H23 0.9500 . ? C24 C25 1.354(8) . ? C24 H24 0.9500 . ? C25 C26 1.387(7) . ? C25 H25 0.9500 . ? C26 C27 1.465(7) . ? C27 C28 1.381(7) . ? C28 C29 1.357(8) . ? C28 H28 0.9500 . ? C29 C30 1.347(9) . ? C29 H29 0.9500 . ? C30 C31 1.391(8) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? Cl1 O3 1.302(12) . ? Cl1 O4 1.339(13) . ? Cl1 O6 1.389(17) . ? Cl1 O5 1.430(16) . ? Cl2 O7 1.371(6) . ? Cl2 O7 1.371(6) 2_655 ? Cl2 O8 1.403(4) . ? Cl2 O8 1.403(4) 2_655 ? 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 N6 Ru N8 96.01(17) . . ? N6 Ru N7 97.54(18) . . ? N8 Ru N7 78.96(17) . . ? N6 Ru N1 167.25(17) . . ? N8 Ru N1 95.73(18) . . ? N7 Ru N1 89.58(16) . . ? N6 Ru N5 78.7(2) . . ? N8 Ru N5 101.13(18) . . ? N7 Ru N5 176.2(2) . . ? N1 Ru N5 94.2(2) . . ? N6 Ru O1 88.85(17) . . ? N8 Ru O1 172.56(17) . . ? N7 Ru O1 94.86(16) . . ? N1 Ru O1 79.99(18) . . ? N5 Ru O1 85.32(15) . . ? C3 N1 C2 108.4(5) . . ? C3 N1 Ru 140.6(5) . . ? C2 N1 Ru 110.9(4) . . ? C4 N2 C3 105.8(5) . . ? C4 N2 H2 127.1 . . ? C3 N2 H2 127.1 . . ? C5 N3 C11 105.3(5) . . ? C5 N3 H3 127.3 . . ? C11 N3 H3 127.3 . . ? C5 N4 C6 103.2(5) . . ? C12 N5 C16 119.6(6) . . ? C12 N5 Ru 126.1(5) . . ? C16 N5 Ru 113.9(4) . . ? C21 N6 C17 117.9(5) . . ? C21 N6 Ru 125.8(4) . . ? C17 N6 Ru 116.2(5) . . ? C22 N7 C26 119.2(5) . . ? C22 N7 Ru 124.8(4) . . ? C26 N7 Ru 115.9(3) . . ? C31 N8 C27 118.5(5) . . ? C31 N8 Ru 125.9(4) . . ? C27 N8 Ru 115.4(3) . . ? C1 O1 Ru 115.6(4) . . ? O1 C1 O2 124.3(6) . . ? O1 C1 C2 116.7(6) . . ? O2 C1 C2 119.1(7) . . ? C4 C2 N1 105.2(5) . . ? C4 C2 C1 138.0(6) . . ? N1 C2 C1 116.7(6) . . ? N1 C3 N2 111.0(5) . . ? N1 C3 H3A 124.5 . . ? N2 C3 H3A 124.5 . . ? N2 C4 C2 109.6(6) . . ? N2 C4 C5 120.1(6) . . ? C2 C4 C5 130.3(6) . . ? N4 C5 N3 116.0(6) . . ? N4 C5 C4 124.5(6) . . ? N3 C5 C4 119.5(6) . . ? N4 C6 C11 111.0(6) . . ? N4 C6 C7 130.0(7) . . ? C11 C6 C7 119.0(6) . . ? C8 C7 C6 117.8(6) . . ? C8 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? C7 C8 C9 121.3(7) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C10 C9 C8 121.0(6) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 118.1(7) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? C10 C11 C6 122.8(7) . . ? C10 C11 N3 132.7(7) . . ? C6 C11 N3 104.5(5) . . ? N5 C12 C13 121.9(8) . . ? N5 C12 H12 119.0 . . ? C13 C12 H12 119.0 . . ? C14 C13 C12 118.0(10) . . ? C14 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? C13 C14 C15 122.3(9) . . ? C13 C14 H14 118.8 . . ? C15 C14 H14 118.8 . . ? C14 C15 C16 117.9(8) . . ? C14 C15 H15 121.0 . . ? C16 C15 H15 121.0 . . ? N5 C16 C15 120.1(7) . . ? N5 C16 C17 115.2(6) . . ? C15 C16 C17 124.7(8) . . ? N6 C17 C18 121.0(6) . . ? N6 C17 C16 114.4(6) . . ? C18 C17 C16 124.6(6) . . ? C19 C18 C17 119.8(7) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 119.3(7) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C19 C20 C21 119.1(7) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? N6 C21 C20 122.9(6) . . ? N6 C21 H21 118.5 . . ? C20 C21 H21 118.5 . . ? N7 C22 C23 121.1(5) . . ? N7 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C24 C23 C22 120.1(6) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 118.1(6) . . ? C25 C24 H24 121.0 . . ? C23 C24 H24 121.0 . . ? C24 C25 C26 121.5(5) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.2 . . ? N7 C26 C25 119.9(5) . . ? N7 C26 C27 113.9(4) . . ? C25 C26 C27 126.1(5) . . ? N8 C27 C28 121.1(5) . . ? N8 C27 C26 115.3(4) . . ? C28 C27 C26 123.6(5) . . ? C29 C28 C27 119.7(6) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C30 C29 C28 119.7(6) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 119.4(6) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? N8 C31 C30 121.5(6) . . ? N8 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? O3 Cl1 O4 119.1(13) . . ? O3 Cl1 O6 94.1(17) . . ? O4 Cl1 O6 114.2(14) . . ? O3 Cl1 O5 119.2(15) . . ? O4 Cl1 O5 103.6(16) . . ? O6 Cl1 O5 106.0(19) . . ? O7 Cl2 O7 110.5(7) . 2_655 ? O7 Cl2 O8 110.5(4) . . ? O7 Cl2 O8 108.6(3) 2_655 . ? O7 Cl2 O8 108.6(3) . 2_655 ? O7 Cl2 O8 110.5(4) 2_655 2_655 ? O8 Cl2 O8 108.1(4) . 2_655 ? 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 N6 Ru N1 C3 -147.6(8) . . . . ? N8 Ru N1 C3 9.3(7) . . . . ? N7 Ru N1 C3 88.2(6) . . . . ? N5 Ru N1 C3 -92.3(6) . . . . ? O1 Ru N1 C3 -176.8(7) . . . . ? N6 Ru N1 C2 26.6(9) . . . . ? N8 Ru N1 C2 -176.5(3) . . . . ? N7 Ru N1 C2 -97.6(3) . . . . ? N5 Ru N1 C2 81.9(3) . . . . ? O1 Ru N1 C2 -2.6(3) . . . . ? N6 Ru N5 C12 -176.1(5) . . . . ? N8 Ru N5 C12 -82.1(5) . . . . ? N7 Ru N5 C12 -173(2) . . . . ? N1 Ru N5 C12 14.6(5) . . . . ? O1 Ru N5 C12 94.2(5) . . . . ? N6 Ru N5 C16 11.5(3) . . . . ? N8 Ru N5 C16 105.5(4) . . . . ? N7 Ru N5 C16 15(3) . . . . ? N1 Ru N5 C16 -157.8(4) . . . . ? O1 Ru N5 C16 -78.2(4) . . . . ? N8 Ru N6 C21 75.3(4) . . . . ? N7 Ru N6 C21 -4.3(4) . . . . ? N1 Ru N6 C21 -127.8(8) . . . . ? N5 Ru N6 C21 175.5(5) . . . . ? O1 Ru N6 C21 -99.1(4) . . . . ? N8 Ru N6 C17 -109.4(3) . . . . ? N7 Ru N6 C17 171.0(3) . . . . ? N1 Ru N6 C17 47.5(9) . . . . ? N5 Ru N6 C17 -9.2(3) . . . . ? O1 Ru N6 C17 76.2(3) . . . . ? N6 Ru N7 C22 -80.8(4) . . . . ? N8 Ru N7 C22 -175.5(5) . . . . ? N1 Ru N7 C22 88.6(4) . . . . ? N5 Ru N7 C22 -84(3) . . . . ? O1 Ru N7 C22 8.7(4) . . . . ? N6 Ru N7 C26 99.0(4) . . . . ? N8 Ru N7 C26 4.3(4) . . . . ? N1 Ru N7 C26 -91.6(4) . . . . ? N5 Ru N7 C26 96(3) . . . . ? O1 Ru N7 C26 -171.5(4) . . . . ? N6 Ru N8 C31 81.9(5) . . . . ? N7 Ru N8 C31 178.4(5) . . . . ? N1 Ru N8 C31 -93.1(5) . . . . ? N5 Ru N8 C31 2.3(5) . . . . ? O1 Ru N8 C31 -147.5(13) . . . . ? N6 Ru N8 C27 -102.8(4) . . . . ? N7 Ru N8 C27 -6.3(4) . . . . ? N1 Ru N8 C27 82.1(4) . . . . ? N5 Ru N8 C27 177.5(4) . . . . ? O1 Ru N8 C27 27.7(16) . . . . ? N6 Ru O1 C1 -173.2(4) . . . . ? N8 Ru O1 C1 55.9(15) . . . . ? N7 Ru O1 C1 89.4(4) . . . . ? N1 Ru O1 C1 0.6(4) . . . . ? N5 Ru O1 C1 -94.4(4) . . . . ? Ru O1 C1 O2 -178.8(4) . . . . ? Ru O1 C1 C2 1.5(6) . . . . ? C3 N1 C2 C4 -0.3(6) . . . . ? Ru N1 C2 C4 -176.4(3) . . . . ? C3 N1 C2 C1 -179.6(5) . . . . ? Ru N1 C2 C1 4.3(5) . . . . ? O1 C1 C2 C4 177.0(6) . . . . ? O2 C1 C2 C4 -2.6(10) . . . . ? O1 C1 C2 N1 -4.0(7) . . . . ? O2 C1 C2 N1 176.4(4) . . . . ? C2 N1 C3 N2 0.2(6) . . . . ? Ru N1 C3 N2 174.5(4) . . . . ? C4 N2 C3 N1 0.0(6) . . . . ? C3 N2 C4 C2 -0.2(6) . . . . ? C3 N2 C4 C5 -179.8(5) . . . . ? N1 C2 C4 N2 0.3(6) . . . . ? C1 C2 C4 N2 179.4(6) . . . . ? N1 C2 C4 C5 179.9(5) . . . . ? C1 C2 C4 C5 -1.1(11) . . . . ? C6 N4 C5 N3 -0.6(6) . . . . ? C6 N4 C5 C4 177.2(5) . . . . ? C11 N3 C5 N4 0.4(6) . . . . ? C11 N3 C5 C4 -177.5(4) . . . . ? N2 C4 C5 N4 3.8(8) . . . . ? C2 C4 C5 N4 -175.8(6) . . . . ? N2 C4 C5 N3 -178.5(5) . . . . ? C2 C4 C5 N3 2.0(9) . . . . ? C5 N4 C6 C11 0.6(6) . . . . ? C5 N4 C6 C7 179.5(6) . . . . ? N4 C6 C7 C8 179.5(5) . . . . ? C11 C6 C7 C8 -1.6(8) . . . . ? C6 C7 C8 C9 2.0(9) . . . . ? C7 C8 C9 C10 -1.6(10) . . . . ? C8 C9 C10 C11 0.9(10) . . . . ? C9 C10 C11 C6 -0.5(9) . . . . ? C9 C10 C11 N3 179.9(6) . . . . ? N4 C6 C11 C10 180.0(5) . . . . ? C7 C6 C11 C10 1.0(9) . . . . ? N4 C6 C11 N3 -0.3(6) . . . . ? C7 C6 C11 N3 -179.4(5) . . . . ? C5 N3 C11 C10 179.6(6) . . . . ? C5 N3 C11 C6 0.0(5) . . . . ? C16 N5 C12 C13 3.0(8) . . . . ? Ru N5 C12 C13 -169.0(4) . . . . ? N5 C12 C13 C14 0.5(10) . . . . ? C12 C13 C14 C15 -1.8(12) . . . . ? C13 C14 C15 C16 -0.4(11) . . . . ? C12 N5 C16 C15 -5.4(8) . . . . ? Ru N5 C16 C15 167.6(4) . . . . ? C12 N5 C16 C17 174.9(4) . . . . ? Ru N5 C16 C17 -12.2(6) . . . . ? C14 C15 C16 N5 4.1(8) . . . . ? C14 C15 C16 C17 -176.2(5) . . . . ? C21 N6 C17 C18 0.1(7) . . . . ? Ru N6 C17 C18 -175.6(4) . . . . ? C21 N6 C17 C16 -178.8(5) . . . . ? Ru N6 C17 C16 5.5(5) . . . . ? N5 C16 C17 N6 4.6(7) . . . . ? C15 C16 C17 N6 -175.2(5) . . . . ? N5 C16 C17 C18 -174.3(5) . . . . ? C15 C16 C17 C18 5.9(8) . . . . ? N6 C17 C18 C19 -0.9(9) . . . . ? C16 C17 C18 C19 178.0(6) . . . . ? C17 C18 C19 C20 0.4(10) . . . . ? C18 C19 C20 C21 0.8(10) . . . . ? C17 N6 C21 C20 1.2(8) . . . . ? Ru N6 C21 C20 176.4(4) . . . . ? C19 C20 C21 N6 -1.6(9) . . . . ? C26 N7 C22 C23 2.7(8) . . . . ? Ru N7 C22 C23 -177.5(5) . . . . ? N7 C22 C23 C24 -2.8(10) . . . . ? C22 C23 C24 C25 1.5(10) . . . . ? C23 C24 C25 C26 -0.3(9) . . . . ? C22 N7 C26 C25 -1.4(7) . . . . ? Ru N7 C26 C25 178.8(4) . . . . ? C22 N7 C26 C27 178.1(5) . . . . ? Ru N7 C26 C27 -1.8(5) . . . . ? C24 C25 C26 N7 0.2(8) . . . . ? C24 C25 C26 C27 -179.2(5) . . . . ? C31 N8 C27 C28 3.4(8) . . . . ? Ru N8 C27 C28 -172.3(4) . . . . ? C31 N8 C27 C26 -177.1(5) . . . . ? Ru N8 C27 C26 7.3(6) . . . . ? N7 C26 C27 N8 -3.6(6) . . . . ? C25 C26 C27 N8 175.8(5) . . . . ? N7 C26 C27 C28 175.9(5) . . . . ? C25 C26 C27 C28 -4.6(8) . . . . ? N8 C27 C28 C29 -2.9(8) . . . . ? C26 C27 C28 C29 177.6(5) . . . . ? C27 C28 C29 C30 0.7(9) . . . . ? C28 C29 C30 C31 0.8(10) . . . . ? C27 N8 C31 C30 -1.8(9) . . . . ? Ru N8 C31 C30 173.4(5) . . . . ? C29 C30 C31 N8 -0.3(10) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.735 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.065 data_1 _database_code_depnum_ccdc_archive 'CCDC 839295' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H59 N21 O4 Ru2' _chemical_formula_weight 1484.54 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.7216(3) _cell_length_b 22.8856(7) _cell_length_c 12.4104(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.881(3) _cell_angle_gamma 90.00 _cell_volume 3317.09(17) _cell_formula_units_Z 2 _cell_measurement_reflns_used 17574 _cell_measurement_theta_min 3.4064 _cell_measurement_theta_max 32.8454 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_absorpt_coefficient_mu 0.524 _exptl_absorpt_correction_T_min 0.8420 _exptl_absorpt_correction_T_max 0.8935 _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 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _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 24270 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 24.99 _reflns_number_total 11620 _reflns_number_gt 9981 _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^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.27(2) _refine_ls_number_reflns 11620 _refine_ls_number_parameters 906 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 -0.55091(3) -0.014074(15) 1.79309(3) 0.02060(9) Uani 1 1 d . . . Ru2 Ru 0.00778(3) -1.059440(14) 1.33643(3) 0.01967(9) Uani 1 1 d . . . O1 O -0.4937(3) -0.04644(14) 1.6486(2) 0.0243(8) Uani 1 1 d . . . O2 O -0.3764(3) -0.11111(16) 1.5812(3) 0.0300(8) Uani 1 1 d . . . O3 O -0.0462(3) -1.02681(13) 1.4829(3) 0.0237(8) Uani 1 1 d . . . O4 O -0.1536(3) -0.96083(15) 1.5573(3) 0.0288(8) Uani 1 1 d . . . N1 N -0.4362(4) -0.07693(19) 1.8497(3) 0.0220(10) Uani 1 1 d . . . N2 N -0.3190(4) -0.14394(19) 1.9324(3) 0.0265(10) Uani 1 1 d . . . N3 N -0.2227(3) -0.18949(18) 1.6694(3) 0.0248(9) Uani 1 1 d . . . N4 N -0.1625(4) -0.22387(19) 1.8340(3) 0.0303(10) Uani 1 1 d . . . N5 N -0.6859(4) -0.07091(19) 1.7677(3) 0.0226(10) Uani 1 1 d . . . N6 N -0.6760(3) 0.04011(19) 1.7234(3) 0.0222(10) Uani 1 1 d . . . N7 N -0.4169(3) 0.04231(19) 1.8184(3) 0.0202(10) Uani 1 1 d . . . N8 N -0.5828(3) 0.02180(17) 1.9365(3) 0.0251(9) Uani 1 1 d . . . N9 N -0.1077(4) -0.99556(19) 1.2836(3) 0.0194(10) Uani 1 1 d . . . N10 N -0.2336(4) -0.93091(19) 1.2042(3) 0.0260(10) Uani 1 1 d . . . N11 N -0.3064(3) -0.88269(18) 1.4730(3) 0.0248(9) Uani 1 1 d . . . N13 N 0.1432(4) -1.00298(18) 1.3610(3) 0.0206(10) Uani 1 1 d . . . N14 N 0.1332(4) -1.11386(18) 1.4032(3) 0.0205(10) Uani 1 1 d . . . N15 N 0.0361(3) -1.09252(16) 1.1904(3) 0.0205(9) Uani 1 1 d . . . N16 N -0.1262(4) -1.11568(18) 1.3137(3) 0.0204(10) Uani 1 1 d . . . C1 C -0.4178(4) -0.0884(2) 1.6572(4) 0.0213(10) Uani 1 1 d . . . C2 C -0.3840(4) -0.1059(2) 1.7729(4) 0.0225(11) Uani 1 1 d . . . C3 C -0.3949(4) -0.1011(2) 1.9436(4) 0.0261(11) Uani 1 1 d . . . H3 H -0.4175 -0.0889 2.0118 0.031 Uiso 1 1 calc R . . C4 C -0.3123(4) -0.1472(2) 1.8235(4) 0.0236(11) Uani 1 1 d . . . C5 C -0.2332(4) -0.1882(2) 1.7785(4) 0.0261(11) Uani 1 1 d . . . C6 C -0.1019(4) -0.2510(2) 1.7570(4) 0.0300(12) Uani 1 1 d . . . C7 C -0.0128(4) -0.2907(2) 1.7700(5) 0.0380(13) Uani 1 1 d . . . H7 H 0.0154 -0.3043 1.8395 0.046 Uiso 1 1 calc R . . C8 C 0.0345(5) -0.3104(3) 1.6750(5) 0.0442(15) Uani 1 1 d . . . H8 H 0.0953 -0.3379 1.6810 0.053 Uiso 1 1 calc R . . C9 C -0.0054(4) -0.2904(2) 1.5751(5) 0.0370(14) Uani 1 1 d . . . H9 H 0.0284 -0.3046 1.5134 0.044 Uiso 1 1 calc R . . C10 C -0.0940(4) -0.2499(2) 1.5607(4) 0.0304(12) Uani 1 1 d . . . H10 H -0.1215 -0.2365 1.4908 0.036 Uiso 1 1 calc R . . C11 C -0.1402(4) -0.2301(2) 1.6529(4) 0.0274(12) Uani 1 1 d . . . C12 C -0.6830(4) -0.1291(2) 1.7892(4) 0.0257(12) Uani 1 1 d . . . H12 H -0.6171 -0.1447 1.8288 0.031 Uiso 1 1 calc R . . C13 C -0.7697(5) -0.1661(2) 1.7567(4) 0.0288(12) Uani 1 1 d . . . H13 H -0.7643 -0.2065 1.7738 0.035 Uiso 1 1 calc R . . C14 C -0.8655(5) -0.1443(3) 1.6990(5) 0.0327(14) Uani 1 1 d . . . H14 H -0.9268 -0.1695 1.6752 0.039 Uiso 1 1 calc R . . C15 C -0.8720(4) -0.0854(2) 1.6758(4) 0.0292(13) Uani 1 1 d . . . H15 H -0.9377 -0.0696 1.6362 0.035 Uiso 1 1 calc R . . C16 C -0.7814(4) -0.0499(2) 1.7112(4) 0.0241(12) Uani 1 1 d . . . C17 C -0.7793(4) 0.0140(2) 1.6936(4) 0.0239(12) Uani 1 1 d . . . C18 C -0.8722(4) 0.0460(3) 1.6536(4) 0.0287(13) Uani 1 1 d . . . H18 H -0.9430 0.0271 1.6335 0.034 Uiso 1 1 calc R . . C19 C -0.8627(5) 0.1052(3) 1.6427(5) 0.0348(14) Uani 1 1 d . . . H19 H -0.9264 0.1278 1.6143 0.042 Uiso 1 1 calc R . . C20 C -0.7593(5) 0.1320(2) 1.6735(5) 0.0337(13) Uani 1 1 d . . . H20 H -0.7516 0.1731 1.6676 0.040 Uiso 1 1 calc R . . C21 C -0.6687(4) 0.0988(2) 1.7124(4) 0.0257(12) Uani 1 1 d . . . H21 H -0.5977 0.1175 1.7325 0.031 Uiso 1 1 calc R . . C22 C -0.3371(4) 0.0532(2) 1.7492(4) 0.0262(11) Uani 1 1 d . . . H22 H -0.3475 0.0380 1.6779 0.031 Uiso 1 1 calc R . . C23 C -0.2404(4) 0.0859(2) 1.7788(4) 0.0288(12) Uani 1 1 d . . . H23 H -0.1856 0.0930 1.7282 0.035 Uiso 1 1 calc R . . C24 C -0.2237(4) 0.1082(2) 1.8818(4) 0.0279(12) Uani 1 1 d . . . H24 H -0.1573 0.1305 1.9035 0.033 Uiso 1 1 calc R . . C25 C -0.3053(4) 0.0975(2) 1.9530(4) 0.0272(12) Uani 1 1 d . . . H25 H -0.2959 0.1128 2.0243 0.033 Uiso 1 1 calc R . . C26 C -0.4012(4) 0.0645(2) 1.9203(4) 0.0223(11) Uani 1 1 d . . . C27 C -0.4965(4) 0.0539(2) 1.9864(4) 0.0216(10) Uani 1 1 d . . . C28 C -0.5065(4) 0.0783(2) 2.0866(4) 0.0271(11) Uani 1 1 d . . . H28 H -0.4434 0.0984 2.1227 0.033 Uiso 1 1 calc R . . C29 C -0.6076(5) 0.0737(3) 2.1343(5) 0.0331(14) Uani 1 1 d . . . H29 H -0.6157 0.0908 2.2031 0.040 Uiso 1 1 calc R . . C30 C -0.6980(4) 0.0436(2) 2.0800(4) 0.0300(12) Uani 1 1 d . . . H30 H -0.7704 0.0419 2.1087 0.036 Uiso 1 1 calc R . . C31 C -0.6813(4) 0.0167(2) 1.9857(4) 0.0264(11) Uani 1 1 d . . . H31 H -0.7412 -0.0067 1.9524 0.032 Uiso 1 1 calc R . . C32 C -0.1190(4) -0.9849(2) 1.4741(4) 0.0234(11) Uani 1 1 d . . . C33 C -0.1577(4) -0.9676(2) 1.3641(4) 0.0203(10) Uani 1 1 d . . . C34 C -0.1549(4) -0.9736(2) 1.1907(4) 0.0262(12) Uani 1 1 d . . . H34 H -0.1356 -0.9864 1.1218 0.031 Uiso 1 1 calc R . . C35 C -0.2351(4) -0.9269(2) 1.3143(4) 0.0220(11) Uani 1 1 d . . . C36 C -0.3125(4) -0.8880(2) 1.3619(4) 0.0210(11) Uani 1 1 d . . . C37 C -0.4467(4) -0.8286(2) 1.3936(4) 0.0206(10) Uani 1 1 d . . . C38 C -0.5414(4) -0.7910(2) 1.3887(4) 0.0277(12) Uani 1 1 d . . . H38 H -0.5777 -0.7788 1.3210 0.033 Uiso 1 1 calc R . . C39 C -0.5800(4) -0.7722(2) 1.4834(4) 0.0308(12) Uani 1 1 d . . . H39 H -0.6449 -0.7472 1.4813 0.037 Uiso 1 1 calc R . . C40 C -0.5256(4) -0.7891(2) 1.5843(4) 0.0296(12) Uani 1 1 d . . . H40 H -0.5548 -0.7753 1.6488 0.035 Uiso 1 1 calc R . . C41 C -0.4320(4) -0.8249(2) 1.5916(4) 0.0253(11) Uani 1 1 d . . . H41 H -0.3941 -0.8355 1.6595 0.030 Uiso 1 1 calc R . . C42 C -0.3948(4) -0.8449(2) 1.4948(4) 0.0221(11) Uani 1 1 d . . . C43 C 0.1399(4) -0.9455(2) 1.3416(4) 0.0242(11) Uani 1 1 d . . . H43 H 0.0735 -0.9297 1.3031 0.029 Uiso 1 1 calc R . . C44 C 0.2288(5) -0.9080(3) 1.3751(5) 0.0317(14) Uani 1 1 d . . . H44 H 0.2243 -0.8676 1.3574 0.038 Uiso 1 1 calc R . . C45 C 0.3234(4) -0.9300(2) 1.4340(4) 0.0279(12) Uani 1 1 d . . . H45 H 0.3844 -0.9049 1.4598 0.034 Uiso 1 1 calc R . . C46 C 0.3284(4) -0.9890(2) 1.4553(4) 0.0263(13) Uani 1 1 d . . . H46 H 0.3938 -1.0050 1.4952 0.032 Uiso 1 1 calc R . . C47 C 0.2387(4) -1.0253(2) 1.4186(4) 0.0226(12) Uani 1 1 d . . . C48 C 0.2347(5) -1.0879(3) 1.4358(4) 0.0235(13) Uani 1 1 d . . . C49 C 0.3289(4) -1.1204(2) 1.4797(4) 0.0276(12) Uani 1 1 d . . . H49 H 0.3991 -1.1017 1.5028 0.033 Uiso 1 1 calc R . . C50 C 0.3174(5) -1.1804(3) 1.4885(4) 0.0299(13) Uani 1 1 d . . . H50 H 0.3804 -1.2032 1.5176 0.036 Uiso 1 1 calc R . . C51 C 0.2152(5) -1.2070(2) 1.4554(4) 0.0324(13) Uani 1 1 d . . . H51 H 0.2069 -1.2482 1.4612 0.039 Uiso 1 1 calc R . . C52 C 0.1247(4) -1.1729(2) 1.4134(4) 0.0253(12) Uani 1 1 d . . . H52 H 0.0540 -1.1913 1.3910 0.030 Uiso 1 1 calc R . . C53 C 0.1311(4) -1.0870(2) 1.1419(4) 0.0250(11) Uani 1 1 d . . . H53 H 0.1929 -1.0654 1.1769 0.030 Uiso 1 1 calc R . . C54 C 0.1446(4) -1.1121(2) 1.0385(4) 0.0306(12) Uani 1 1 d . . . H54 H 0.2119 -1.1054 1.0029 0.037 Uiso 1 1 calc R . . C55 C 0.0580(5) -1.1460(2) 0.9924(4) 0.0289(12) Uani 1 1 d . . . H55 H 0.0655 -1.1639 0.9243 0.035 Uiso 1 1 calc R . . C56 C -0.0406(4) -1.1544(2) 1.0442(4) 0.0264(11) Uani 1 1 d . . . H56 H -0.1016 -1.1775 1.0120 0.032 Uiso 1 1 calc R . . C57 C -0.0485(4) -1.1282(2) 1.1450(4) 0.0254(11) Uani 1 1 d . . . C58 C -0.1428(4) -1.1393(2) 1.2111(4) 0.0234(11) Uani 1 1 d . . . C59 C -0.2397(4) -1.1713(2) 1.1790(4) 0.0248(12) Uani 1 1 d . . . H59 H -0.2494 -1.1873 1.1082 0.030 Uiso 1 1 calc R . . C60 C -0.3221(4) -1.1800(2) 1.2499(4) 0.0284(12) Uani 1 1 d . . . H60 H -0.3894 -1.2018 1.2289 0.034 Uiso 1 1 calc R . . C61 C -0.3047(4) -1.1561(2) 1.3535(4) 0.0257(12) Uani 1 1 d . . . H61 H -0.3603 -1.1614 1.4041 0.031 Uiso 1 1 calc R . . C62 C -0.2064(4) -1.1249(2) 1.3818(4) 0.0246(11) Uani 1 1 d . . . H62 H -0.1952 -1.1092 1.4528 0.030 Uiso 1 1 calc R . . C111 C -0.1073(5) -0.0425(3) 1.8210(6) 0.0533(18) Uani 1 1 d . . . H11A H -0.1274 -0.0248 1.7501 0.080 Uiso 1 1 calc R . . H11B H -0.1767 -0.0480 1.8585 0.080 Uiso 1 1 calc R . . H11C H -0.0708 -0.0805 1.8114 0.080 Uiso 1 1 calc R . . C222 C -0.0286(5) -0.0046(3) 1.8845(5) 0.0448(15) Uani 1 1 d . . . C333 C -0.4372(5) -0.0274(3) 1.3108(5) 0.0469(16) Uani 1 1 d . . . H33A H -0.3615 -0.0319 1.2839 0.070 Uiso 1 1 calc R . . H33B H -0.4337 -0.0395 1.3867 0.070 Uiso 1 1 calc R . . H33C H -0.4608 0.0137 1.3048 0.070 Uiso 1 1 calc R . . C444 C -0.5196(5) -0.0635(3) 1.2470(5) 0.0437(14) Uani 1 1 d . . . C555 C -0.1311(7) -0.3209(3) 2.0745(7) 0.073(2) Uani 1 1 d . . . H55A H -0.1090 -0.3048 2.0061 0.110 Uiso 1 1 calc R . . H55B H -0.2092 -0.3086 2.0857 0.110 Uiso 1 1 calc R . . H55C H -0.1278 -0.3637 2.0719 0.110 Uiso 1 1 calc R . . C666 C -0.0549(6) -0.3003(3) 2.1608(6) 0.0543(17) Uani 1 1 d . . . C777 C -0.5329(7) -0.7713(3) 2.0842(5) 0.067(2) Uani 1 1 d . . . H77A H -0.6069 -0.7793 2.1125 0.100 Uiso 1 1 calc R . . H77B H -0.5143 -0.7298 2.0938 0.100 Uiso 1 1 calc R . . H77C H -0.4733 -0.7950 2.1233 0.100 Uiso 1 1 calc R . . C888 C -0.5394(6) -0.7858(3) 1.9700(6) 0.0509(16) Uani 1 1 d . . . C999 C 0.2830(6) -0.2314(3) 2.1794(5) 0.0587(18) Uani 1 1 d . . . H99A H 0.3088 -0.1909 2.1890 0.088 Uiso 1 1 calc R . . H99B H 0.3401 -0.2577 2.2154 0.088 Uiso 1 1 calc R . . H99C H 0.2098 -0.2364 2.2110 0.088 Uiso 1 1 calc R . . C110 C 0.2683(6) -0.2453(3) 2.0634(6) 0.0603(18) Uani 1 1 d . . . N111 N 0.0322(5) 0.0260(3) 1.9349(6) 0.0660(18) Uani 1 1 d . . . N222 N -0.5812(5) -0.0925(3) 1.1965(6) 0.0667(18) Uani 1 1 d . . . N333 N 0.0037(6) -0.2840(3) 2.2285(7) 0.081(2) Uani 1 1 d . . . N444 N -0.5450(5) -0.7980(2) 1.8805(5) 0.0582(15) Uani 1 1 d . . . N555 N 0.2564(7) -0.2551(3) 1.9739(5) 0.089(2) Uani 1 1 d . . . N12 N -0.3944(3) -0.85574(19) 1.3115(3) 0.0269(9) Uani 1 1 d . . . H3N H -0.267(4) -0.165(2) 1.619(4) 0.020(12) Uiso 1 1 d . . . H11N H -0.263(8) -0.898(4) 1.543(8) 0.13(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02018(18) 0.0217(2) 0.01944(18) -0.00192(17) -0.00110(15) 0.00153(16) Ru2 0.01873(18) 0.02050(19) 0.01944(18) -0.00158(17) -0.00039(14) 0.00119(16) O1 0.0284(18) 0.029(2) 0.0145(16) -0.0002(14) -0.0059(14) 0.0012(15) O2 0.034(2) 0.036(2) 0.0201(18) -0.0021(17) 0.0006(16) 0.0093(17) O3 0.0220(16) 0.024(2) 0.0243(17) -0.0018(15) -0.0012(14) 0.0027(15) O4 0.0329(19) 0.035(2) 0.0188(17) -0.0072(16) 0.0018(15) 0.0097(16) N1 0.017(2) 0.031(3) 0.017(2) -0.0058(18) -0.0009(17) 0.0002(17) N2 0.028(2) 0.027(3) 0.024(2) 0.0033(19) -0.0003(19) 0.0048(19) N3 0.023(2) 0.021(2) 0.029(2) -0.0011(19) -0.0019(19) 0.0034(18) N4 0.028(2) 0.027(2) 0.034(2) -0.0022(19) -0.005(2) 0.0055(18) N5 0.024(2) 0.025(3) 0.020(2) -0.0017(19) 0.0012(18) 0.0051(17) N6 0.021(2) 0.024(2) 0.021(2) -0.0033(19) -0.0007(19) 0.0034(18) N7 0.018(2) 0.023(2) 0.019(2) 0.0028(19) -0.0030(18) 0.0034(18) N8 0.023(2) 0.020(2) 0.032(2) 0.0017(18) -0.0013(19) 0.0003(18) N9 0.017(2) 0.022(2) 0.019(2) -0.0040(17) 0.0006(17) 0.0010(16) N10 0.027(2) 0.024(2) 0.026(2) 0.003(2) -0.0010(19) 0.0060(19) N11 0.023(2) 0.029(2) 0.022(2) -0.0013(18) -0.0003(18) 0.0042(18) N13 0.023(2) 0.020(3) 0.019(2) -0.0035(18) 0.0036(18) -0.0003(17) N14 0.023(2) 0.022(2) 0.017(2) -0.0037(19) 0.0071(18) -0.0019(18) N15 0.022(2) 0.019(2) 0.020(2) -0.0017(17) 0.0012(17) 0.0030(17) N16 0.025(2) 0.018(2) 0.018(2) -0.0010(18) 0.0009(19) 0.0062(18) C1 0.024(2) 0.021(3) 0.019(2) -0.003(2) -0.004(2) 0.004(2) C2 0.017(2) 0.028(3) 0.021(2) 0.001(2) -0.001(2) 0.002(2) C3 0.028(3) 0.024(3) 0.026(3) -0.001(2) 0.002(2) -0.001(2) C4 0.027(3) 0.023(3) 0.020(3) 0.000(2) -0.001(2) 0.003(2) C5 0.026(3) 0.027(3) 0.025(3) 0.000(2) -0.002(2) -0.001(2) C6 0.030(3) 0.024(3) 0.035(3) -0.004(2) -0.003(2) -0.003(2) C7 0.034(3) 0.035(3) 0.044(3) -0.001(3) -0.005(3) 0.013(2) C8 0.027(3) 0.032(3) 0.073(5) -0.012(3) 0.000(3) 0.005(2) C9 0.024(3) 0.033(3) 0.055(4) -0.018(3) 0.011(3) -0.001(2) C10 0.026(3) 0.029(3) 0.037(3) -0.008(2) 0.003(2) -0.004(2) C11 0.023(3) 0.023(3) 0.037(3) -0.008(2) 0.003(2) -0.004(2) C12 0.026(3) 0.025(3) 0.026(3) -0.003(2) 0.001(2) 0.000(2) C13 0.033(3) 0.030(3) 0.024(3) 0.003(2) 0.008(2) -0.004(2) C14 0.031(3) 0.034(4) 0.034(3) -0.009(3) 0.007(3) -0.012(3) C15 0.022(3) 0.038(3) 0.027(3) -0.003(2) 0.000(2) 0.000(2) C16 0.021(2) 0.035(4) 0.016(2) -0.005(2) 0.0010(19) -0.001(2) C17 0.023(3) 0.030(3) 0.019(3) -0.003(2) 0.002(2) -0.005(2) C18 0.022(3) 0.038(4) 0.026(3) -0.004(2) -0.002(2) -0.002(2) C19 0.037(3) 0.033(3) 0.033(3) 0.003(3) -0.008(3) 0.007(3) C20 0.038(3) 0.025(3) 0.037(3) 0.007(3) 0.000(3) 0.001(3) C21 0.026(3) 0.023(3) 0.027(3) -0.004(2) 0.000(2) 0.001(2) C22 0.030(3) 0.024(3) 0.024(3) 0.003(2) 0.000(2) 0.004(2) C23 0.020(3) 0.028(3) 0.038(3) 0.005(2) 0.005(2) 0.001(2) C24 0.025(3) 0.030(3) 0.028(3) 0.003(2) -0.003(2) -0.003(2) C25 0.025(3) 0.028(3) 0.027(3) -0.004(2) -0.004(2) 0.003(2) C26 0.023(3) 0.021(3) 0.023(3) 0.000(2) 0.002(2) 0.005(2) C27 0.023(2) 0.015(2) 0.027(3) 0.000(2) 0.001(2) 0.0019(19) C28 0.030(3) 0.031(3) 0.019(2) 0.002(2) -0.004(2) -0.001(2) C29 0.036(3) 0.036(3) 0.028(3) 0.000(3) 0.010(3) 0.001(3) C30 0.029(3) 0.031(3) 0.031(3) 0.004(2) 0.008(2) 0.002(2) C31 0.021(3) 0.030(3) 0.029(3) -0.001(2) 0.005(2) 0.001(2) C32 0.018(2) 0.020(3) 0.031(3) -0.001(2) 0.000(2) -0.002(2) C33 0.016(2) 0.023(3) 0.022(2) -0.005(2) 0.001(2) -0.001(2) C34 0.026(3) 0.029(3) 0.024(3) 0.000(2) 0.005(2) 0.004(2) C35 0.020(2) 0.026(3) 0.019(2) -0.004(2) -0.001(2) -0.003(2) C36 0.021(2) 0.019(3) 0.022(2) -0.002(2) 0.001(2) -0.003(2) C37 0.018(2) 0.019(3) 0.024(2) -0.001(2) -0.001(2) 0.0006(19) C38 0.028(3) 0.028(3) 0.026(3) 0.000(2) -0.004(2) 0.001(2) C39 0.022(2) 0.023(3) 0.048(3) -0.002(2) 0.002(2) 0.006(2) C40 0.036(3) 0.025(3) 0.028(3) -0.003(2) 0.007(2) -0.002(2) C41 0.028(3) 0.024(3) 0.024(3) 0.004(2) 0.002(2) 0.005(2) C42 0.018(2) 0.019(3) 0.029(3) 0.000(2) 0.002(2) 0.0002(19) C43 0.027(3) 0.023(3) 0.022(3) 0.002(2) 0.001(2) 0.001(2) C44 0.032(3) 0.027(3) 0.036(3) -0.002(3) 0.004(3) -0.009(3) C45 0.028(3) 0.029(3) 0.026(3) 0.000(2) 0.002(2) -0.009(2) C46 0.018(3) 0.037(3) 0.023(3) -0.005(2) 0.000(2) -0.003(2) C47 0.019(2) 0.029(4) 0.019(2) -0.009(2) 0.002(2) 0.001(2) C48 0.021(3) 0.031(3) 0.018(3) -0.004(2) 0.002(2) 0.001(2) C49 0.024(3) 0.035(3) 0.023(3) -0.004(2) 0.001(2) 0.004(2) C50 0.025(3) 0.036(4) 0.028(3) 0.006(3) 0.001(2) 0.011(2) C51 0.037(3) 0.026(3) 0.035(3) 0.000(2) 0.005(3) 0.008(2) C52 0.027(3) 0.025(3) 0.024(3) 0.000(2) -0.001(2) 0.002(2) C53 0.028(3) 0.021(3) 0.026(3) -0.003(2) 0.000(2) 0.000(2) C54 0.029(3) 0.037(3) 0.026(3) -0.006(2) 0.008(2) 0.000(2) C55 0.040(3) 0.030(3) 0.018(2) -0.005(2) 0.004(2) 0.006(2) C56 0.029(3) 0.026(3) 0.024(3) -0.008(2) 0.001(2) -0.001(2) C57 0.025(3) 0.029(3) 0.021(3) 0.007(2) -0.001(2) 0.003(2) C58 0.025(3) 0.025(3) 0.020(3) -0.002(2) -0.004(2) 0.003(2) C59 0.026(3) 0.025(3) 0.023(3) -0.002(2) 0.002(2) 0.001(2) C60 0.024(3) 0.026(3) 0.034(3) 0.002(2) -0.004(2) -0.006(2) C61 0.026(3) 0.029(3) 0.023(3) 0.006(2) 0.004(2) -0.002(2) C62 0.026(3) 0.025(3) 0.023(3) -0.002(2) 0.002(2) 0.002(2) C111 0.038(3) 0.039(4) 0.080(5) 0.005(3) -0.007(3) 0.007(3) C222 0.024(3) 0.048(4) 0.062(4) 0.008(3) 0.000(3) 0.005(3) C333 0.037(3) 0.042(4) 0.062(4) -0.005(3) 0.004(3) -0.007(3) C444 0.029(3) 0.043(3) 0.058(4) 0.006(4) 0.003(3) -0.002(3) C555 0.088(6) 0.054(5) 0.079(5) 0.010(4) 0.012(5) -0.001(4) C666 0.051(4) 0.046(4) 0.066(5) 0.008(4) 0.009(4) 0.000(3) C777 0.101(6) 0.051(4) 0.050(4) -0.009(3) 0.016(4) 0.015(4) C888 0.059(4) 0.040(4) 0.051(4) 0.004(3) -0.009(3) 0.006(3) C999 0.071(5) 0.054(4) 0.050(4) 0.008(3) 0.000(4) 0.003(4) C110 0.076(5) 0.049(4) 0.055(4) 0.007(3) 0.001(4) 0.022(3) N111 0.034(3) 0.060(4) 0.102(5) -0.003(4) -0.004(3) 0.001(3) N222 0.041(3) 0.056(4) 0.100(5) -0.003(4) -0.006(3) -0.002(3) N333 0.065(4) 0.060(4) 0.119(6) 0.014(4) 0.008(4) -0.014(4) N444 0.079(4) 0.048(3) 0.045(3) 0.005(3) -0.014(3) -0.005(3) N555 0.146(7) 0.066(4) 0.054(4) 0.006(3) 0.003(4) 0.049(4) N12 0.026(2) 0.030(2) 0.024(2) -0.0022(18) -0.0052(18) 0.0007(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N8 2.023(4) . ? Ru1 N7 2.037(4) . ? Ru1 N5 2.052(4) . ? Ru1 N1 2.052(4) . ? Ru1 N6 2.054(4) . ? Ru1 O1 2.103(3) . ? Ru2 N15 2.018(4) . ? Ru2 N16 2.032(4) . ? Ru2 N14 2.047(4) . ? Ru2 N13 2.049(4) . ? Ru2 N9 2.061(4) . ? Ru2 O3 2.111(3) . ? O1 C1 1.307(5) . ? O2 C1 1.214(5) . ? O3 C32 1.282(5) . ? O4 C32 1.267(6) . ? N1 C3 1.343(7) . ? N1 C2 1.350(6) . ? N2 C3 1.340(7) . ? N2 C4 1.362(6) . ? N3 C11 1.369(6) . ? N3 C5 1.370(6) . ? N3 H3N 0.95(5) . ? N4 C5 1.315(6) . ? N4 C6 1.384(7) . ? N5 C16 1.358(6) . ? N5 C12 1.358(7) . ? N6 C21 1.354(7) . ? N6 C17 1.372(6) . ? N7 C22 1.346(6) . ? N7 C26 1.360(6) . ? N8 C31 1.356(6) . ? N8 C27 1.357(6) . ? N9 C34 1.334(7) . ? N9 C33 1.361(6) . ? N10 C34 1.363(7) . ? N10 C35 1.371(6) . ? N11 C36 1.379(6) . ? N11 C42 1.394(6) . ? N11 H11N 1.03(10) . ? N13 C43 1.336(7) . ? N13 C47 1.374(6) . ? N14 C48 1.360(7) . ? N14 C52 1.361(6) . ? N15 C53 1.316(6) . ? N15 C57 1.368(6) . ? N16 C62 1.332(6) . ? N16 C58 1.382(6) . ? C1 C2 1.511(6) . ? C2 C4 1.379(7) . ? C3 H3 0.9500 . ? C4 C5 1.465(7) . ? C6 C7 1.384(7) . ? C6 C11 1.415(7) . ? C7 C8 1.417(8) . ? C7 H7 0.9500 . ? C8 C9 1.366(8) . ? C8 H8 0.9500 . ? C9 C10 1.392(8) . ? C9 H9 0.9500 . ? C10 C11 1.383(7) . ? C10 H10 0.9500 . ? C12 C13 1.357(7) . ? C12 H12 0.9500 . ? C13 C14 1.373(8) . ? C13 H13 0.9500 . ? C14 C15 1.377(8) . ? C14 H14 0.9500 . ? C15 C16 1.379(7) . ? C15 H15 0.9500 . ? C16 C17 1.479(7) . ? C17 C18 1.370(7) . ? C18 C19 1.369(8) . ? C18 H18 0.9500 . ? C19 C20 1.382(8) . ? C19 H19 0.9500 . ? C20 C21 1.360(7) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.381(7) . ? C22 H22 0.9500 . ? C23 C24 1.375(7) . ? C23 H23 0.9500 . ? C24 C25 1.377(7) . ? C24 H24 0.9500 . ? C25 C26 1.386(7) . ? C25 H25 0.9500 . ? C26 C27 1.462(7) . ? C27 C28 1.377(7) . ? C28 C29 1.374(7) . ? C28 H28 0.9500 . ? C29 C30 1.389(8) . ? C29 H29 0.9500 . ? C30 C31 1.350(7) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.457(7) . ? C33 C35 1.405(7) . ? C34 H34 0.9500 . ? C35 C36 1.435(7) . ? C36 N12 1.325(6) . ? C37 N12 1.381(6) . ? C37 C42 1.399(7) . ? C37 C38 1.403(7) . ? C38 C39 1.365(7) . ? C38 H38 0.9500 . ? C39 C40 1.411(7) . ? C39 H39 0.9500 . ? C40 C41 1.365(7) . ? C40 H40 0.9500 . ? C41 C42 1.391(7) . ? C41 H41 0.9500 . ? C43 C44 1.387(7) . ? C43 H43 0.9500 . ? C44 C45 1.370(8) . ? C44 H44 0.9500 . ? C45 C46 1.378(8) . ? C45 H45 0.9500 . ? C46 C47 1.386(7) . ? C46 H46 0.9500 . ? C47 C48 1.451(7) . ? C48 C49 1.402(7) . ? C49 C50 1.384(8) . ? C49 H49 0.9500 . ? C50 C51 1.376(8) . ? C50 H50 0.9500 . ? C51 C52 1.383(7) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.426(7) . ? C53 H53 0.9500 . ? C54 C55 1.365(7) . ? C54 H54 0.9500 . ? C55 C56 1.383(7) . ? C55 H55 0.9500 . ? C56 C57 1.398(7) . ? C56 H56 0.9500 . ? C57 C58 1.454(7) . ? C58 C59 1.381(7) . ? C59 C60 1.375(7) . ? C59 H59 0.9500 . ? C60 C61 1.396(7) . ? C60 H60 0.9500 . ? C61 C62 1.377(7) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C111 C222 1.450(9) . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C222 N111 1.146(8) . ? C333 C444 1.454(9) . ? C333 H33A 0.9800 . ? C333 H33B 0.9800 . ? C333 H33C 0.9800 . ? C444 N222 1.131(8) . ? C555 C666 1.415(11) . ? C555 H55A 0.9800 . ? C555 H55B 0.9800 . ? C555 H55C 0.9800 . ? C666 N333 1.104(9) . ? C777 C888 1.451(9) . ? C777 H77A 0.9800 . ? C777 H77B 0.9800 . ? C777 H77C 0.9800 . ? C888 N444 1.141(8) . ? C999 C110 1.469(9) . ? C999 H99A 0.9800 . ? C999 H99B 0.9800 . ? C999 H99C 0.9800 . ? C110 N555 1.131(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Ru1 N7 78.76(16) . . ? N8 Ru1 N5 101.21(16) . . ? N7 Ru1 N5 180.0(2) . . ? N8 Ru1 N1 98.52(16) . . ? N7 Ru1 N1 85.23(15) . . ? N5 Ru1 N1 94.74(18) . . ? N8 Ru1 N6 86.94(16) . . ? N7 Ru1 N6 101.31(18) . . ? N5 Ru1 N6 78.72(15) . . ? N1 Ru1 N6 172.25(18) . . ? N8 Ru1 O1 171.69(15) . . ? N7 Ru1 O1 93.26(15) . . ? N5 Ru1 O1 86.77(14) . . ? N1 Ru1 O1 78.32(14) . . ? N6 Ru1 O1 96.99(14) . . ? N15 Ru2 N16 79.76(16) . . ? N15 Ru2 N14 88.14(15) . . ? N16 Ru2 N14 101.01(18) . . ? N15 Ru2 N13 100.68(15) . . ? N16 Ru2 N13 179.41(18) . . ? N14 Ru2 N13 78.63(15) . . ? N15 Ru2 N9 97.71(16) . . ? N16 Ru2 N9 85.76(15) . . ? N14 Ru2 N9 171.79(18) . . ? N13 Ru2 N9 94.56(18) . . ? N15 Ru2 O3 172.05(14) . . ? N16 Ru2 O3 93.36(14) . . ? N14 Ru2 O3 97.15(14) . . ? N13 Ru2 O3 86.22(14) . . ? N9 Ru2 O3 77.66(14) . . ? C1 O1 Ru1 117.0(3) . . ? C32 O3 Ru2 115.9(3) . . ? C3 N1 C2 105.1(4) . . ? C3 N1 Ru1 139.7(3) . . ? C2 N1 Ru1 115.2(3) . . ? C3 N2 C4 103.7(4) . . ? C11 N3 C5 106.6(4) . . ? C11 N3 H3N 130(3) . . ? C5 N3 H3N 124(3) . . ? C5 N4 C6 104.7(4) . . ? C16 N5 C12 117.1(5) . . ? C16 N5 Ru1 116.5(4) . . ? C12 N5 Ru1 125.8(3) . . ? C21 N6 C17 117.8(4) . . ? C21 N6 Ru1 126.3(3) . . ? C17 N6 Ru1 115.6(3) . . ? C22 N7 C26 118.5(4) . . ? C22 N7 Ru1 126.0(4) . . ? C26 N7 Ru1 114.9(3) . . ? C31 N8 C27 118.0(4) . . ? C31 N8 Ru1 126.2(3) . . ? C27 N8 Ru1 115.8(3) . . ? C34 N9 C33 106.5(4) . . ? C34 N9 Ru2 139.1(4) . . ? C33 N9 Ru2 114.3(3) . . ? C34 N10 C35 103.7(4) . . ? C36 N11 C42 105.8(4) . . ? C36 N11 H11N 142(5) . . ? C42 N11 H11N 112(5) . . ? C43 N13 C47 117.9(4) . . ? C43 N13 Ru2 125.7(4) . . ? C47 N13 Ru2 115.4(3) . . ? C48 N14 C52 118.3(5) . . ? C48 N14 Ru2 115.8(4) . . ? C52 N14 Ru2 125.9(4) . . ? C53 N15 C57 118.8(4) . . ? C53 N15 Ru2 125.8(3) . . ? C57 N15 Ru2 115.1(3) . . ? C62 N16 C58 118.1(4) . . ? C62 N16 Ru2 126.2(3) . . ? C58 N16 Ru2 115.0(3) . . ? O2 C1 O1 124.4(4) . . ? O2 C1 C2 122.4(4) . . ? O1 C1 C2 113.2(4) . . ? N1 C2 C4 108.0(4) . . ? N1 C2 C1 116.3(4) . . ? C4 C2 C1 135.6(4) . . ? N2 C3 N1 113.8(4) . . ? N2 C3 H3 123.1 . . ? N1 C3 H3 123.1 . . ? N2 C4 C2 109.3(4) . . ? N2 C4 C5 120.3(4) . . ? C2 C4 C5 130.3(5) . . ? N4 C5 N3 113.5(5) . . ? N4 C5 C4 126.2(5) . . ? N3 C5 C4 120.2(4) . . ? C7 C6 N4 129.8(5) . . ? C7 C6 C11 120.4(5) . . ? N4 C6 C11 109.7(4) . . ? C6 C7 C8 117.1(5) . . ? C6 C7 H7 121.4 . . ? C8 C7 H7 121.4 . . ? C9 C8 C7 121.4(5) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C10 122.2(5) . . ? C8 C9 H9 118.9 . . ? C10 C9 H9 118.9 . . ? C11 C10 C9 116.9(5) . . ? C11 C10 H10 121.6 . . ? C9 C10 H10 121.6 . . ? N3 C11 C10 132.7(5) . . ? N3 C11 C6 105.4(4) . . ? C10 C11 C6 121.9(5) . . ? C13 C12 N5 123.2(5) . . ? C13 C12 H12 118.4 . . ? N5 C12 H12 118.4 . . ? C12 C13 C14 119.1(5) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C13 C14 C15 119.5(5) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C16 118.9(5) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? N5 C16 C15 122.2(5) . . ? N5 C16 C17 113.8(5) . . ? C15 C16 C17 124.0(5) . . ? C18 C17 N6 121.5(5) . . ? C18 C17 C16 123.9(5) . . ? N6 C17 C16 114.6(5) . . ? C19 C18 C17 119.7(5) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 119.2(5) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C21 C20 C19 119.5(5) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? N6 C21 C20 122.3(5) . . ? N6 C21 H21 118.8 . . ? C20 C21 H21 118.8 . . ? N7 C22 C23 122.0(5) . . ? N7 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C24 C23 C22 119.8(5) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 118.6(5) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.7 . . ? C24 C25 C26 120.0(5) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? N7 C26 C25 121.2(5) . . ? N7 C26 C27 114.2(4) . . ? C25 C26 C27 124.4(5) . . ? N8 C27 C28 121.0(5) . . ? N8 C27 C26 114.1(4) . . ? C28 C27 C26 124.5(5) . . ? C29 C28 C27 120.1(5) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 118.6(5) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? C31 C30 C29 119.1(5) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C30 C31 N8 122.9(5) . . ? C30 C31 H31 118.5 . . ? N8 C31 H31 118.5 . . ? O4 C32 O3 120.8(4) . . ? O4 C32 C33 123.4(4) . . ? O3 C32 C33 115.8(4) . . ? N9 C33 C35 106.9(4) . . ? N9 C33 C32 116.2(4) . . ? C35 C33 C32 136.9(4) . . ? N9 C34 N10 113.5(4) . . ? N9 C34 H34 123.2 . . ? N10 C34 H34 123.2 . . ? N10 C35 C33 109.4(4) . . ? N10 C35 C36 120.9(4) . . ? C33 C35 C36 129.6(4) . . ? N12 C36 N11 113.4(4) . . ? N12 C36 C35 127.5(4) . . ? N11 C36 C35 119.0(4) . . ? N12 C37 C42 110.9(4) . . ? N12 C37 C38 130.0(4) . . ? C42 C37 C38 119.0(4) . . ? C39 C38 C37 118.4(5) . . ? C39 C38 H38 120.8 . . ? C37 C38 H38 120.8 . . ? C38 C39 C40 121.3(5) . . ? C38 C39 H39 119.3 . . ? C40 C39 H39 119.3 . . ? C41 C40 C39 121.6(5) . . ? C41 C40 H40 119.2 . . ? C39 C40 H40 119.2 . . ? C40 C41 C42 116.7(5) . . ? C40 C41 H41 121.6 . . ? C42 C41 H41 121.6 . . ? C41 C42 N11 131.8(5) . . ? C41 C42 C37 122.9(4) . . ? N11 C42 C37 105.3(4) . . ? N13 C43 C44 123.1(5) . . ? N13 C43 H43 118.5 . . ? C44 C43 H43 118.5 . . ? C45 C44 C43 119.1(6) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? C44 C45 C46 118.8(5) . . ? C44 C45 H45 120.6 . . ? C46 C45 H45 120.6 . . ? C45 C46 C47 120.4(5) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? N13 C47 C46 120.7(5) . . ? N13 C47 C48 114.1(5) . . ? C46 C47 C48 125.2(5) . . ? N14 C48 C49 121.6(5) . . ? N14 C48 C47 115.2(5) . . ? C49 C48 C47 123.2(5) . . ? C50 C49 C48 118.6(5) . . ? C50 C49 H49 120.7 . . ? C48 C49 H49 120.7 . . ? C51 C50 C49 120.3(5) . . ? C51 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? C50 C51 C52 118.8(5) . . ? C50 C51 H51 120.6 . . ? C52 C51 H51 120.6 . . ? N14 C52 C51 122.4(5) . . ? N14 C52 H52 118.8 . . ? C51 C52 H52 118.8 . . ? N15 C53 C54 122.4(5) . . ? N15 C53 H53 118.8 . . ? C54 C53 H53 118.8 . . ? C55 C54 C53 118.1(5) . . ? C55 C54 H54 120.9 . . ? C53 C54 H54 120.9 . . ? C54 C55 C56 120.3(5) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C55 C56 C57 118.6(5) . . ? C55 C56 H56 120.7 . . ? C57 C56 H56 120.7 . . ? N15 C57 C56 121.5(4) . . ? N15 C57 C58 115.6(4) . . ? C56 C57 C58 122.7(5) . . ? C59 C58 N16 121.4(5) . . ? C59 C58 C57 125.2(5) . . ? N16 C58 C57 113.4(4) . . ? C60 C59 C58 119.9(5) . . ? C60 C59 H59 120.1 . . ? C58 C59 H59 120.1 . . ? C59 C60 C61 118.5(5) . . ? C59 C60 H60 120.8 . . ? C61 C60 H60 120.8 . . ? C62 C61 C60 119.5(5) . . ? C62 C61 H61 120.3 . . ? C60 C61 H61 120.3 . . ? N16 C62 C61 122.7(5) . . ? N16 C62 H62 118.6 . . ? C61 C62 H62 118.6 . . ? C222 C111 H11A 109.5 . . ? C222 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C222 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? N111 C222 C111 179.0(7) . . ? C444 C333 H33A 109.5 . . ? C444 C333 H33B 109.5 . . ? H33A C333 H33B 109.5 . . ? C444 C333 H33C 109.5 . . ? H33A C333 H33C 109.5 . . ? H33B C333 H33C 109.5 . . ? N222 C444 C333 178.0(7) . . ? C666 C555 H55A 109.5 . . ? C666 C555 H55B 109.5 . . ? H55A C555 H55B 109.5 . . ? C666 C555 H55C 109.5 . . ? H55A C555 H55C 109.5 . . ? H55B C555 H55C 109.5 . . ? N333 C666 C555 179.4(9) . . ? 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 . . ? N444 C888 C777 179.0(8) . . ? C110 C999 H99A 109.5 . . ? C110 C999 H99B 109.5 . . ? H99A C999 H99B 109.5 . . ? C110 C999 H99C 109.5 . . ? H99A C999 H99C 109.5 . . ? H99B C999 H99C 109.5 . . ? N555 C110 C999 178.9(7) . . ? C36 N12 C37 104.5(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 N8 Ru1 O1 C1 68.6(11) . . . . ? N7 Ru1 O1 C1 84.6(3) . . . . ? N5 Ru1 O1 C1 -95.4(3) . . . . ? N1 Ru1 O1 C1 0.2(3) . . . . ? N6 Ru1 O1 C1 -173.6(3) . . . . ? N15 Ru2 O3 C32 -56.0(11) . . . . ? N16 Ru2 O3 C32 -85.9(3) . . . . ? N14 Ru2 O3 C32 172.6(3) . . . . ? N13 Ru2 O3 C32 94.5(3) . . . . ? N9 Ru2 O3 C32 -1.0(3) . . . . ? N8 Ru1 N1 C3 9.9(6) . . . . ? N7 Ru1 N1 C3 87.7(6) . . . . ? N5 Ru1 N1 C3 -92.2(6) . . . . ? N6 Ru1 N1 C3 -124.6(12) . . . . ? O1 Ru1 N1 C3 -177.9(6) . . . . ? N8 Ru1 N1 C2 -172.0(3) . . . . ? N7 Ru1 N1 C2 -94.2(4) . . . . ? N5 Ru1 N1 C2 85.9(4) . . . . ? N6 Ru1 N1 C2 53.5(15) . . . . ? O1 Ru1 N1 C2 0.2(3) . . . . ? N8 Ru1 N5 C16 91.2(3) . . . . ? N7 Ru1 N5 C16 140(100) . . . . ? N1 Ru1 N5 C16 -169.1(3) . . . . ? N6 Ru1 N5 C16 6.6(3) . . . . ? O1 Ru1 N5 C16 -91.2(3) . . . . ? N8 Ru1 N5 C12 -98.3(4) . . . . ? N7 Ru1 N5 C12 -49(100) . . . . ? N1 Ru1 N5 C12 1.4(4) . . . . ? N6 Ru1 N5 C12 177.1(4) . . . . ? O1 Ru1 N5 C12 79.4(4) . . . . ? N8 Ru1 N6 C21 70.8(4) . . . . ? N7 Ru1 N6 C21 -7.1(4) . . . . ? N5 Ru1 N6 C21 172.9(4) . . . . ? N1 Ru1 N6 C21 -154.1(11) . . . . ? O1 Ru1 N6 C21 -101.8(4) . . . . ? N8 Ru1 N6 C17 -103.6(3) . . . . ? N7 Ru1 N6 C17 178.5(3) . . . . ? N5 Ru1 N6 C17 -1.5(3) . . . . ? N1 Ru1 N6 C17 31.4(15) . . . . ? O1 Ru1 N6 C17 83.8(3) . . . . ? N8 Ru1 N7 C22 -175.6(4) . . . . ? N5 Ru1 N7 C22 135(100) . . . . ? N1 Ru1 N7 C22 84.8(4) . . . . ? N6 Ru1 N7 C22 -91.0(4) . . . . ? O1 Ru1 N7 C22 6.8(4) . . . . ? N8 Ru1 N7 C26 13.1(3) . . . . ? N5 Ru1 N7 C26 -36(100) . . . . ? N1 Ru1 N7 C26 -86.6(4) . . . . ? N6 Ru1 N7 C26 97.6(4) . . . . ? O1 Ru1 N7 C26 -164.6(3) . . . . ? N7 Ru1 N8 C31 167.9(4) . . . . ? N5 Ru1 N8 C31 -12.2(4) . . . . ? N1 Ru1 N8 C31 -108.8(4) . . . . ? N6 Ru1 N8 C31 65.7(4) . . . . ? O1 Ru1 N8 C31 -175.8(8) . . . . ? N7 Ru1 N8 C27 -11.9(3) . . . . ? N5 Ru1 N8 C27 168.1(3) . . . . ? N1 Ru1 N8 C27 71.5(3) . . . . ? N6 Ru1 N8 C27 -114.0(3) . . . . ? O1 Ru1 N8 C27 4.4(12) . . . . ? N15 Ru2 N9 C34 -3.6(6) . . . . ? N16 Ru2 N9 C34 -82.6(6) . . . . ? N14 Ru2 N9 C34 131.6(11) . . . . ? N13 Ru2 N9 C34 97.9(5) . . . . ? O3 Ru2 N9 C34 -177.0(6) . . . . ? N15 Ru2 N9 C33 172.5(3) . . . . ? N16 Ru2 N9 C33 93.4(3) . . . . ? N14 Ru2 N9 C33 -52.3(14) . . . . ? N13 Ru2 N9 C33 -86.1(4) . . . . ? O3 Ru2 N9 C33 -0.9(3) . . . . ? N15 Ru2 N13 C43 97.5(4) . . . . ? N16 Ru2 N13 C43 -124(18) . . . . ? N14 Ru2 N13 C43 -176.6(4) . . . . ? N9 Ru2 N13 C43 -1.3(4) . . . . ? O3 Ru2 N13 C43 -78.6(4) . . . . ? N15 Ru2 N13 C47 -93.9(3) . . . . ? N16 Ru2 N13 C47 44(19) . . . . ? N14 Ru2 N13 C47 -8.0(3) . . . . ? N9 Ru2 N13 C47 167.4(3) . . . . ? O3 Ru2 N13 C47 90.1(3) . . . . ? N15 Ru2 N14 C48 105.4(3) . . . . ? N16 Ru2 N14 C48 -175.4(3) . . . . ? N13 Ru2 N14 C48 4.1(3) . . . . ? N9 Ru2 N14 C48 -30.3(14) . . . . ? O3 Ru2 N14 C48 -80.6(3) . . . . ? N15 Ru2 N14 C52 -72.0(4) . . . . ? N16 Ru2 N14 C52 7.2(4) . . . . ? N13 Ru2 N14 C52 -173.3(4) . . . . ? N9 Ru2 N14 C52 152.3(11) . . . . ? O3 Ru2 N14 C52 102.0(4) . . . . ? N16 Ru2 N15 C53 -166.5(4) . . . . ? N14 Ru2 N15 C53 -64.9(4) . . . . ? N13 Ru2 N15 C53 13.1(4) . . . . ? N9 Ru2 N15 C53 109.3(4) . . . . ? O3 Ru2 N15 C53 163.1(9) . . . . ? N16 Ru2 N15 C57 7.0(3) . . . . ? N14 Ru2 N15 C57 108.6(3) . . . . ? N13 Ru2 N15 C57 -173.4(3) . . . . ? N9 Ru2 N15 C57 -77.2(3) . . . . ? O3 Ru2 N15 C57 -23.4(12) . . . . ? N15 Ru2 N16 C62 -179.9(4) . . . . ? N14 Ru2 N16 C62 94.0(4) . . . . ? N13 Ru2 N16 C62 42(19) . . . . ? N9 Ru2 N16 C62 -81.3(4) . . . . ? O3 Ru2 N16 C62 -3.9(4) . . . . ? N15 Ru2 N16 C58 -10.0(3) . . . . ? N14 Ru2 N16 C58 -96.0(4) . . . . ? N13 Ru2 N16 C58 -148(18) . . . . ? N9 Ru2 N16 C58 88.7(4) . . . . ? O3 Ru2 N16 C58 166.0(3) . . . . ? Ru1 O1 C1 O2 -179.5(4) . . . . ? Ru1 O1 C1 C2 -0.4(5) . . . . ? C3 N1 C2 C4 0.1(5) . . . . ? Ru1 N1 C2 C4 -178.6(3) . . . . ? C3 N1 C2 C1 178.3(4) . . . . ? Ru1 N1 C2 C1 -0.4(5) . . . . ? O2 C1 C2 N1 179.7(5) . . . . ? O1 C1 C2 N1 0.5(6) . . . . ? O2 C1 C2 C4 -2.8(9) . . . . ? O1 C1 C2 C4 178.1(5) . . . . ? C4 N2 C3 N1 -0.3(6) . . . . ? C2 N1 C3 N2 0.1(6) . . . . ? Ru1 N1 C3 N2 178.3(4) . . . . ? C3 N2 C4 C2 0.4(6) . . . . ? C3 N2 C4 C5 177.6(5) . . . . ? N1 C2 C4 N2 -0.3(6) . . . . ? C1 C2 C4 N2 -178.0(5) . . . . ? N1 C2 C4 C5 -177.2(5) . . . . ? C1 C2 C4 C5 5.1(10) . . . . ? C6 N4 C5 N3 -0.6(6) . . . . ? C6 N4 C5 C4 -176.7(5) . . . . ? C11 N3 C5 N4 1.3(6) . . . . ? C11 N3 C5 C4 177.7(4) . . . . ? N2 C4 C5 N4 -1.1(8) . . . . ? C2 C4 C5 N4 175.5(5) . . . . ? N2 C4 C5 N3 -176.9(5) . . . . ? C2 C4 C5 N3 -0.3(8) . . . . ? C5 N4 C6 C7 176.8(6) . . . . ? C5 N4 C6 C11 -0.3(6) . . . . ? N4 C6 C7 C8 -178.7(5) . . . . ? C11 C6 C7 C8 -1.9(8) . . . . ? C6 C7 C8 C9 0.6(8) . . . . ? C7 C8 C9 C10 0.1(9) . . . . ? C8 C9 C10 C11 0.4(8) . . . . ? C5 N3 C11 C10 179.9(5) . . . . ? C5 N3 C11 C6 -1.4(5) . . . . ? C9 C10 C11 N3 176.8(5) . . . . ? C9 C10 C11 C6 -1.7(7) . . . . ? C7 C6 C11 N3 -176.4(5) . . . . ? N4 C6 C11 N3 1.1(6) . . . . ? C7 C6 C11 C10 2.5(8) . . . . ? N4 C6 C11 C10 180.0(4) . . . . ? C16 N5 C12 C13 0.2(7) . . . . ? Ru1 N5 C12 C13 -170.3(4) . . . . ? N5 C12 C13 C14 0.2(8) . . . . ? C12 C13 C14 C15 -0.4(8) . . . . ? C13 C14 C15 C16 0.2(8) . . . . ? C12 N5 C16 C15 -0.4(7) . . . . ? Ru1 N5 C16 C15 170.9(4) . . . . ? C12 N5 C16 C17 178.4(4) . . . . ? Ru1 N5 C16 C17 -10.2(5) . . . . ? C14 C15 C16 N5 0.2(7) . . . . ? C14 C15 C16 C17 -178.5(5) . . . . ? C21 N6 C17 C18 0.2(7) . . . . ? Ru1 N6 C17 C18 175.2(4) . . . . ? C21 N6 C17 C16 -178.2(4) . . . . ? Ru1 N6 C17 C16 -3.3(5) . . . . ? N5 C16 C17 C18 -169.7(4) . . . . ? C15 C16 C17 C18 9.2(9) . . . . ? N5 C16 C17 N6 8.8(6) . . . . ? C15 C16 C17 N6 -172.4(4) . . . . ? N6 C17 C18 C19 0.0(8) . . . . ? C16 C17 C18 C19 178.4(5) . . . . ? C17 C18 C19 C20 -0.7(8) . . . . ? C18 C19 C20 C21 1.0(9) . . . . ? C17 N6 C21 C20 0.1(7) . . . . ? Ru1 N6 C21 C20 -174.2(4) . . . . ? C19 C20 C21 N6 -0.8(8) . . . . ? C26 N7 C22 C23 0.2(7) . . . . ? Ru1 N7 C22 C23 -170.9(4) . . . . ? N7 C22 C23 C24 0.2(8) . . . . ? C22 C23 C24 C25 -0.5(8) . . . . ? C23 C24 C25 C26 0.6(8) . . . . ? C22 N7 C26 C25 -0.2(7) . . . . ? Ru1 N7 C26 C25 171.8(4) . . . . ? C22 N7 C26 C27 175.7(4) . . . . ? Ru1 N7 C26 C27 -12.3(5) . . . . ? C24 C25 C26 N7 -0.2(8) . . . . ? C24 C25 C26 C27 -175.6(5) . . . . ? C31 N8 C27 C28 3.0(7) . . . . ? Ru1 N8 C27 C28 -177.2(4) . . . . ? C31 N8 C27 C26 -170.9(4) . . . . ? Ru1 N8 C27 C26 8.8(5) . . . . ? N7 C26 C27 N8 2.3(6) . . . . ? C25 C26 C27 N8 178.0(5) . . . . ? N7 C26 C27 C28 -171.4(5) . . . . ? C25 C26 C27 C28 4.3(8) . . . . ? N8 C27 C28 C29 -4.3(7) . . . . ? C26 C27 C28 C29 169.0(5) . . . . ? C27 C28 C29 C30 0.7(8) . . . . ? C28 C29 C30 C31 4.2(8) . . . . ? C29 C30 C31 N8 -5.7(8) . . . . ? C27 N8 C31 C30 2.0(7) . . . . ? Ru1 N8 C31 C30 -177.7(4) . . . . ? Ru2 O3 C32 O4 -177.4(3) . . . . ? Ru2 O3 C32 C33 2.6(5) . . . . ? C34 N9 C33 C35 -1.3(5) . . . . ? Ru2 N9 C33 C35 -178.6(3) . . . . ? C34 N9 C33 C32 179.9(4) . . . . ? Ru2 N9 C33 C32 2.6(5) . . . . ? O4 C32 C33 N9 176.5(4) . . . . ? O3 C32 C33 N9 -3.4(6) . . . . ? O4 C32 C33 C35 -1.9(9) . . . . ? O3 C32 C33 C35 178.1(5) . . . . ? C33 N9 C34 N10 1.2(6) . . . . ? Ru2 N9 C34 N10 177.4(4) . . . . ? C35 N10 C34 N9 -0.5(6) . . . . ? C34 N10 C35 C33 -0.3(5) . . . . ? C34 N10 C35 C36 -177.1(4) . . . . ? N9 C33 C35 N10 1.0(5) . . . . ? C32 C33 C35 N10 179.5(5) . . . . ? N9 C33 C35 C36 177.4(5) . . . . ? C32 C33 C35 C36 -4.1(9) . . . . ? C42 N11 C36 N12 1.9(6) . . . . ? C42 N11 C36 C35 -176.9(4) . . . . ? N10 C35 C36 N12 5.4(8) . . . . ? C33 C35 C36 N12 -170.6(5) . . . . ? N10 C35 C36 N11 -176.0(4) . . . . ? C33 C35 C36 N11 8.0(8) . . . . ? N12 C37 C38 C39 176.8(5) . . . . ? C42 C37 C38 C39 -0.8(7) . . . . ? C37 C38 C39 C40 1.1(7) . . . . ? C38 C39 C40 C41 0.1(8) . . . . ? C39 C40 C41 C42 -1.6(7) . . . . ? C40 C41 C42 N11 -177.7(5) . . . . ? C40 C41 C42 C37 1.9(7) . . . . ? C36 N11 C42 C41 178.0(5) . . . . ? C36 N11 C42 C37 -1.6(5) . . . . ? N12 C37 C42 C41 -178.8(4) . . . . ? C38 C37 C42 C41 -0.7(7) . . . . ? N12 C37 C42 N11 0.9(5) . . . . ? C38 C37 C42 N11 178.9(4) . . . . ? C47 N13 C43 C44 1.3(7) . . . . ? Ru2 N13 C43 C44 169.7(4) . . . . ? N13 C43 C44 C45 -2.3(8) . . . . ? C43 C44 C45 C46 1.9(8) . . . . ? C44 C45 C46 C47 -0.8(8) . . . . ? C43 N13 C47 C46 0.0(7) . . . . ? Ru2 N13 C47 C46 -169.6(4) . . . . ? C43 N13 C47 C48 180.0(5) . . . . ? Ru2 N13 C47 C48 10.4(5) . . . . ? C45 C46 C47 N13 -0.2(7) . . . . ? C45 C46 C47 C48 179.8(5) . . . . ? C52 N14 C48 C49 -0.3(7) . . . . ? Ru2 N14 C48 C49 -177.9(4) . . . . ? C52 N14 C48 C47 177.8(5) . . . . ? Ru2 N14 C48 C47 0.2(6) . . . . ? N13 C47 C48 N14 -6.9(7) . . . . ? C46 C47 C48 N14 173.1(4) . . . . ? N13 C47 C48 C49 171.2(4) . . . . ? C46 C47 C48 C49 -8.9(9) . . . . ? N14 C48 C49 C50 0.6(8) . . . . ? C47 C48 C49 C50 -177.3(5) . . . . ? C48 C49 C50 C51 -0.4(8) . . . . ? C49 C50 C51 C52 -0.1(8) . . . . ? C48 N14 C52 C51 -0.2(7) . . . . ? Ru2 N14 C52 C51 177.2(4) . . . . ? C50 C51 C52 N14 0.4(8) . . . . ? C57 N15 C53 C54 6.3(7) . . . . ? Ru2 N15 C53 C54 179.6(4) . . . . ? N15 C53 C54 C55 -4.2(8) . . . . ? C53 C54 C55 C56 1.4(8) . . . . ? C54 C55 C56 C57 -1.0(8) . . . . ? C53 N15 C57 C56 -5.8(7) . . . . ? Ru2 N15 C57 C56 -179.8(4) . . . . ? C53 N15 C57 C58 170.8(4) . . . . ? Ru2 N15 C57 C58 -3.2(5) . . . . ? C55 C56 C57 N15 3.2(7) . . . . ? C55 C56 C57 C58 -173.3(5) . . . . ? C62 N16 C58 C59 0.4(7) . . . . ? Ru2 N16 C58 C59 -170.4(4) . . . . ? C62 N16 C58 C57 -178.1(4) . . . . ? Ru2 N16 C58 C57 11.1(5) . . . . ? N15 C57 C58 C59 176.3(5) . . . . ? C56 C57 C58 C59 -7.1(8) . . . . ? N15 C57 C58 N16 -5.2(6) . . . . ? C56 C57 C58 N16 171.4(4) . . . . ? N16 C58 C59 C60 0.1(8) . . . . ? C57 C58 C59 C60 178.5(5) . . . . ? C58 C59 C60 C61 -0.3(8) . . . . ? C59 C60 C61 C62 -0.1(8) . . . . ? C58 N16 C62 C61 -0.8(7) . . . . ? Ru2 N16 C62 C61 168.9(4) . . . . ? C60 C61 C62 N16 0.6(8) . . . . ? N11 C36 N12 C37 -1.3(5) . . . . ? C35 C36 N12 C37 177.3(5) . . . . ? C42 C37 N12 C36 0.2(5) . . . . ? C38 C37 N12 C36 -177.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.775 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.086