# 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]ClO4 _database_code_depnum_ccdc_archive 'CCDC 904797' #TrackingRef '[1]ClO4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H20 Cl2 N8 O6 Ru' _chemical_formula_weight 592.37 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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.7114(8) _cell_length_b 14.7773(8) _cell_length_c 17.6340(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4354.7(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14055 _cell_measurement_theta_min 3.3446 _cell_measurement_theta_max 32.8420 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 1.019 _exptl_absorpt_correction_T_min 0.7995 _exptl_absorpt_correction_T_max 0.8622 _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 28203 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.0372 _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 -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3826 _reflns_number_gt 2974 _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^)+(0.0778P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3826 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 0.01512(2) 0.32916(2) 0.183755(18) 0.02063(15) Uani 1 1 d . . . Cl1 Cl -0.01250(7) 0.20021(8) 0.26071(6) 0.0337(3) Uani 1 1 d . . . N1 N -0.08908(19) 0.3846(2) 0.21180(19) 0.0251(8) Uani 1 1 d . . . H1 H -0.1318 0.3775 0.1833 0.030 Uiso 1 1 calc R . . N2 N 0.0441(2) 0.4024(2) 0.27309(18) 0.0219(7) Uani 1 1 d . . . H2 H 0.0942 0.4070 0.2879 0.026 Uiso 1 1 calc R . . N3 N 0.1295(2) 0.2809(2) 0.1578(2) 0.0253(8) Uani 1 1 d . . . N4 N 0.1517(2) 0.2771(2) 0.08303(19) 0.0266(8) Uani 1 1 d . . . N5 N 0.0475(2) 0.4301(2) 0.11091(18) 0.0243(7) Uani 1 1 d . . . N6 N 0.08230(19) 0.4084(2) 0.04356(18) 0.0256(8) Uani 1 1 d . . . N7 N -0.02247(19) 0.2599(2) 0.0878(2) 0.0243(8) Uani 1 1 d . . . N8 N 0.02429(19) 0.2646(2) 0.02401(19) 0.0226(7) Uani 1 1 d . . . C1 C -0.0917(2) 0.4323(3) 0.2746(2) 0.0220(9) Uani 1 1 d . . . C2 C -0.1599(3) 0.4754(3) 0.3076(2) 0.0306(10) Uani 1 1 d . . . H2A H -0.2112 0.4691 0.2851 0.037 Uiso 1 1 calc R . . C3 C -0.1505(3) 0.5253(3) 0.3714(2) 0.0320(10) Uani 1 1 d . . . H3 H -0.1959 0.5531 0.3940 0.038 Uiso 1 1 calc R . . C4 C -0.0733(3) 0.5370(3) 0.4055(2) 0.0271(9) Uani 1 1 d . . . H4 H -0.0688 0.5730 0.4499 0.033 Uiso 1 1 calc R . . C5 C -0.0070(3) 0.4987(3) 0.3766(2) 0.0249(9) Uani 1 1 d . . . H5 H 0.0436 0.5077 0.4000 0.030 Uiso 1 1 calc R . . C6 C -0.0140(2) 0.4443(3) 0.3101(2) 0.0218(9) Uani 1 1 d . . . C7 C 0.1948(3) 0.2585(3) 0.1958(3) 0.0330(10) Uani 1 1 d . . . H7 H 0.1979 0.2541 0.2495 0.040 Uiso 1 1 calc R . . C8 C 0.2588(3) 0.2424(3) 0.1461(3) 0.0410(12) Uani 1 1 d . . . H8 H 0.3118 0.2254 0.1593 0.049 Uiso 1 1 calc R . . C9 C 0.2296(2) 0.2558(3) 0.0753(3) 0.0326(11) Uani 1 1 d . . . H9 H 0.2585 0.2512 0.0291 0.039 Uiso 1 1 calc R . . C10 C 0.0501(3) 0.5200(3) 0.1148(2) 0.0278(9) Uani 1 1 d . . . H10 H 0.0286 0.5551 0.1552 0.033 Uiso 1 1 calc R . . C11 C 0.0883(3) 0.5549(3) 0.0519(3) 0.0327(10) Uani 1 1 d . . . H11 H 0.0985 0.6170 0.0416 0.039 Uiso 1 1 calc R . . C12 C 0.1087(3) 0.4826(3) 0.0073(2) 0.0312(10) Uani 1 1 d . . . H12 H 0.1361 0.4845 -0.0398 0.037 Uiso 1 1 calc R . . C13 C -0.0853(2) 0.2104(3) 0.0669(3) 0.0282(10) Uani 1 1 d . . . H13 H -0.1287 0.1957 0.0994 0.034 Uiso 1 1 calc R . . C14 C -0.0797(3) 0.1827(3) -0.0081(3) 0.0307(10) Uani 1 1 d . . . H14 H -0.1167 0.1462 -0.0353 0.037 Uiso 1 1 calc R . . C15 C -0.0096(3) 0.2190(3) -0.0347(3) 0.0281(10) Uani 1 1 d . . . H15 H 0.0112 0.2133 -0.0846 0.034 Uiso 1 1 calc R . . C16 C 0.0981(3) 0.3146(3) 0.0268(2) 0.0265(9) Uani 1 1 d . . . H16 H 0.1245 0.3108 -0.0240 0.032 Uiso 1 1 calc R . . O101 O 0.1483(3) 0.3626(3) -0.1413(2) 0.0695(12) Uani 1 1 d G . . H10A H 0.1184 0.3997 -0.1155 0.104 Uiso 1 1 d G . . H10B H 0.1303 0.3586 -0.1875 0.104 Uiso 1 1 d G . . O102 O 0.1931(3) 0.6233(4) 0.2918(2) 0.1119(19) Uani 1 1 d G . . H10C H 0.2316 0.6168 0.3245 0.168 Uiso 1 1 d G . . H10D H 0.1680 0.5722 0.2864 0.168 Uiso 1 1 d G . . Cl2 Cl 0.21671(6) 0.41158(8) 0.40818(6) 0.0344(3) Uani 1 1 d . . . O111 O 0.15260(19) 0.3565(3) 0.4314(2) 0.0547(10) Uani 1 1 d . . . O222 O 0.29243(17) 0.3692(2) 0.42363(18) 0.0388(8) Uani 1 1 d . . . O333 O 0.2112(2) 0.4262(3) 0.32819(19) 0.0651(13) Uani 1 1 d . . . O444 O 0.2107(2) 0.4965(3) 0.4478(2) 0.0654(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0234(2) 0.0191(2) 0.0193(2) -0.00174(13) 0.00145(13) -0.00001(13) Cl1 0.0435(6) 0.0282(6) 0.0293(6) 0.0066(5) 0.0050(5) -0.0020(5) N1 0.0242(18) 0.0264(19) 0.0246(19) -0.0050(15) -0.0054(15) -0.0007(15) N2 0.0208(16) 0.0234(18) 0.0215(18) 0.0018(14) -0.0008(14) -0.0004(15) N3 0.0282(18) 0.0227(19) 0.0250(19) -0.0034(15) 0.0003(15) 0.0014(15) N4 0.0263(18) 0.0264(19) 0.027(2) -0.0057(15) 0.0029(15) -0.0015(15) N5 0.0296(18) 0.0200(17) 0.0232(18) -0.0019(14) 0.0039(15) 0.0023(15) N6 0.0331(19) 0.0224(18) 0.0214(19) 0.0006(14) 0.0053(15) -0.0008(15) N7 0.0263(18) 0.0235(19) 0.0231(19) -0.0011(15) 0.0040(14) 0.0017(15) N8 0.0269(18) 0.0195(17) 0.0213(19) -0.0042(14) 0.0023(14) -0.0001(14) C1 0.026(2) 0.020(2) 0.019(2) 0.0013(17) 0.0028(16) 0.0046(17) C2 0.028(2) 0.032(2) 0.032(3) -0.0014(19) -0.0027(18) 0.004(2) C3 0.035(2) 0.032(3) 0.028(2) -0.003(2) 0.0057(19) 0.009(2) C4 0.043(3) 0.018(2) 0.019(2) -0.0008(16) 0.0055(19) 0.0015(19) C5 0.035(2) 0.019(2) 0.020(2) -0.0012(17) -0.0028(17) -0.0049(18) C6 0.031(2) 0.013(2) 0.022(2) 0.0027(16) 0.0001(17) -0.0007(17) C7 0.029(2) 0.036(3) 0.034(3) -0.004(2) -0.0046(19) 0.001(2) C8 0.027(2) 0.046(3) 0.050(3) -0.009(2) -0.003(2) 0.002(2) C9 0.026(2) 0.032(3) 0.041(3) -0.010(2) 0.0084(19) -0.002(2) C10 0.033(2) 0.021(2) 0.029(2) -0.0040(18) -0.0019(19) -0.0004(19) C11 0.039(3) 0.021(2) 0.037(3) 0.0014(19) 0.000(2) -0.0052(19) C12 0.034(2) 0.029(2) 0.030(2) 0.0043(19) 0.0019(19) -0.007(2) C13 0.025(2) 0.020(2) 0.040(3) -0.0052(18) 0.0019(19) 0.0044(18) C14 0.026(2) 0.029(2) 0.038(3) -0.015(2) -0.0055(19) 0.0058(18) C15 0.037(2) 0.025(2) 0.023(2) -0.0087(18) -0.0079(19) 0.0073(19) C16 0.034(2) 0.022(2) 0.023(2) -0.0039(17) 0.0076(18) -0.0030(18) O101 0.086(3) 0.078(3) 0.045(2) -0.012(2) 0.014(2) -0.009(3) O102 0.095(4) 0.122(5) 0.118(5) 0.026(4) 0.016(4) 0.002(4) Cl2 0.0259(5) 0.0499(7) 0.0276(6) 0.0037(5) 0.0000(4) -0.0031(5) O111 0.0289(18) 0.071(3) 0.064(3) 0.024(2) 0.0067(17) -0.0100(18) O222 0.0271(16) 0.0425(19) 0.047(2) 0.0028(15) -0.0004(14) 0.0000(15) O333 0.0352(19) 0.135(4) 0.0251(19) 0.016(2) -0.0010(15) -0.014(2) O444 0.054(2) 0.058(3) 0.084(3) -0.025(2) -0.004(2) 0.009(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 1.971(3) . ? Ru1 N1 1.987(3) . ? Ru1 N5 2.041(3) . ? Ru1 N7 2.075(4) . ? Ru1 N3 2.091(3) . ? Ru1 Cl1 2.3844(11) . ? N1 C1 1.313(5) . ? N1 H1 0.8800 . ? N2 C6 1.323(5) . ? N2 H2 0.8800 . ? N3 C7 1.322(5) . ? N3 N4 1.371(5) . ? N4 C9 1.346(5) . ? N4 C16 1.447(5) . ? N5 C10 1.331(5) . ? N5 N6 1.361(4) . ? N6 C12 1.343(5) . ? N6 C16 1.441(5) . ? N7 C13 1.332(5) . ? N7 N8 1.371(5) . ? N8 C15 1.360(5) . ? N8 C16 1.439(5) . ? C1 C2 1.429(6) . ? C1 C6 1.454(5) . ? C2 C3 1.354(6) . ? C2 H2A 0.9500 . ? C3 C4 1.434(6) . ? C3 H3 0.9500 . ? C4 C5 1.344(6) . ? C4 H4 0.9500 . ? C5 C6 1.426(6) . ? C5 H5 0.9500 . ? C7 C8 1.404(6) . ? C7 H7 0.9500 . ? C8 C9 1.355(6) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.381(6) . ? C10 H10 0.9500 . ? C11 C12 1.370(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.387(6) . ? C13 H13 0.9500 . ? C14 C15 1.372(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16 1.0000 . ? O101 H10A 0.8706 . ? O101 H10B 0.8694 . ? O102 H10C 0.8700 . ? O102 H10D 0.8704 . ? Cl2 O111 1.406(3) . ? Cl2 O333 1.430(3) . ? Cl2 O222 1.438(3) . ? Cl2 O444 1.440(4) . ? 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 77.86(13) . . ? N2 Ru1 N5 92.12(13) . . ? N1 Ru1 N5 95.01(13) . . ? N2 Ru1 N7 175.32(13) . . ? N1 Ru1 N7 98.11(13) . . ? N5 Ru1 N7 85.82(13) . . ? N2 Ru1 N3 97.92(13) . . ? N1 Ru1 N3 175.06(13) . . ? N5 Ru1 N3 82.50(13) . . ? N7 Ru1 N3 85.99(13) . . ? N2 Ru1 Cl1 91.79(10) . . ? N1 Ru1 Cl1 91.04(10) . . ? N5 Ru1 Cl1 173.37(9) . . ? N7 Ru1 Cl1 90.66(10) . . ? N3 Ru1 Cl1 91.66(10) . . ? C1 N1 Ru1 117.4(3) . . ? C1 N1 H1 121.3 . . ? Ru1 N1 H1 121.3 . . ? C6 N2 Ru1 118.1(3) . . ? C6 N2 H2 120.9 . . ? Ru1 N2 H2 120.9 . . ? C7 N3 N4 104.8(3) . . ? C7 N3 Ru1 136.7(3) . . ? N4 N3 Ru1 118.1(2) . . ? C9 N4 N3 111.6(3) . . ? C9 N4 C16 128.2(4) . . ? N3 N4 C16 118.4(3) . . ? C10 N5 N6 105.5(3) . . ? C10 N5 Ru1 134.8(3) . . ? N6 N5 Ru1 119.4(2) . . ? C12 N6 N5 111.3(3) . . ? C12 N6 C16 128.8(3) . . ? N5 N6 C16 118.9(3) . . ? C13 N7 N8 104.5(3) . . ? C13 N7 Ru1 137.3(3) . . ? N8 N7 Ru1 118.1(2) . . ? C15 N8 N7 111.2(3) . . ? C15 N8 C16 129.6(4) . . ? N7 N8 C16 119.1(3) . . ? N1 C1 C2 127.6(4) . . ? N1 C1 C6 113.5(3) . . ? C2 C1 C6 118.8(4) . . ? C3 C2 C1 119.3(4) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C2 C3 C4 121.1(4) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 122.2(4) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C4 C5 C6 118.8(4) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? N2 C6 C5 127.6(4) . . ? N2 C6 C1 112.7(4) . . ? C5 C6 C1 119.7(4) . . ? N3 C7 C8 110.7(4) . . ? N3 C7 H7 124.6 . . ? C8 C7 H7 124.6 . . ? C9 C8 C7 106.1(4) . . ? C9 C8 H8 127.0 . . ? C7 C8 H8 127.0 . . ? N4 C9 C8 106.8(4) . . ? N4 C9 H9 126.6 . . ? C8 C9 H9 126.6 . . ? N5 C10 C11 110.3(4) . . ? N5 C10 H10 124.9 . . ? C11 C10 H10 124.9 . . ? C12 C11 C10 106.5(4) . . ? C12 C11 H11 126.7 . . ? C10 C11 H11 126.7 . . ? N6 C12 C11 106.4(4) . . ? N6 C12 H12 126.8 . . ? C11 C12 H12 126.8 . . ? N7 C13 C14 111.9(4) . . ? N7 C13 H13 124.1 . . ? C14 C13 H13 124.1 . . ? C15 C14 C13 105.6(4) . . ? C15 C14 H14 127.2 . . ? C13 C14 H14 127.2 . . ? N8 C15 C14 106.8(4) . . ? N8 C15 H15 126.6 . . ? C14 C15 H15 126.6 . . ? N8 C16 N6 110.2(3) . . ? N8 C16 N4 110.9(3) . . ? N6 C16 N4 110.0(3) . . ? N8 C16 H16 108.6 . . ? N6 C16 H16 108.6 . . ? N4 C16 H16 108.6 . . ? H10A O101 H10B 109.5 . . ? H10C O102 H10D 109.4 . . ? O111 Cl2 O333 109.0(2) . . ? O111 Cl2 O222 111.3(2) . . ? O333 Cl2 O222 108.0(2) . . ? O111 Cl2 O444 108.0(2) . . ? O333 Cl2 O444 110.0(3) . . ? O222 Cl2 O444 110.4(2) . . ? 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 N1 C1 -5.8(3) . . . . ? N5 Ru1 N1 C1 -96.9(3) . . . . ? N7 Ru1 N1 C1 176.6(3) . . . . ? N3 Ru1 N1 C1 -37.4(17) . . . . ? Cl1 Ru1 N1 C1 85.8(3) . . . . ? N1 Ru1 N2 C6 4.8(3) . . . . ? N5 Ru1 N2 C6 99.5(3) . . . . ? N7 Ru1 N2 C6 35.7(17) . . . . ? N3 Ru1 N2 C6 -177.8(3) . . . . ? Cl1 Ru1 N2 C6 -85.9(3) . . . . ? N2 Ru1 N3 C7 32.7(4) . . . . ? N1 Ru1 N3 C7 63.9(17) . . . . ? N5 Ru1 N3 C7 123.9(4) . . . . ? N7 Ru1 N3 C7 -149.8(4) . . . . ? Cl1 Ru1 N3 C7 -59.3(4) . . . . ? N2 Ru1 N3 N4 -139.1(3) . . . . ? N1 Ru1 N3 N4 -108.0(16) . . . . ? N5 Ru1 N3 N4 -48.0(3) . . . . ? N7 Ru1 N3 N4 38.3(3) . . . . ? Cl1 Ru1 N3 N4 128.8(3) . . . . ? C7 N3 N4 C9 -2.1(5) . . . . ? Ru1 N3 N4 C9 172.2(3) . . . . ? C7 N3 N4 C16 -168.3(4) . . . . ? Ru1 N3 N4 C16 6.0(4) . . . . ? N2 Ru1 N5 C10 -28.4(4) . . . . ? N1 Ru1 N5 C10 49.6(4) . . . . ? N7 Ru1 N5 C10 147.4(4) . . . . ? N3 Ru1 N5 C10 -126.1(4) . . . . ? Cl1 Ru1 N5 C10 -154.5(7) . . . . ? N2 Ru1 N5 N6 143.9(3) . . . . ? N1 Ru1 N5 N6 -138.1(3) . . . . ? N7 Ru1 N5 N6 -40.3(3) . . . . ? N3 Ru1 N5 N6 46.2(3) . . . . ? Cl1 Ru1 N5 N6 17.8(11) . . . . ? C10 N5 N6 C12 2.2(5) . . . . ? Ru1 N5 N6 C12 -172.1(3) . . . . ? C10 N5 N6 C16 172.1(3) . . . . ? Ru1 N5 N6 C16 -2.3(5) . . . . ? N2 Ru1 N7 C13 -72.5(17) . . . . ? N1 Ru1 N7 C13 -42.0(4) . . . . ? N5 Ru1 N7 C13 -136.4(4) . . . . ? N3 Ru1 N7 C13 140.8(4) . . . . ? Cl1 Ru1 N7 C13 49.2(4) . . . . ? N2 Ru1 N7 N8 104.4(16) . . . . ? N1 Ru1 N7 N8 134.9(3) . . . . ? N5 Ru1 N7 N8 40.4(3) . . . . ? N3 Ru1 N7 N8 -42.3(3) . . . . ? Cl1 Ru1 N7 N8 -134.0(3) . . . . ? C13 N7 N8 C15 0.2(4) . . . . ? Ru1 N7 N8 C15 -177.6(3) . . . . ? C13 N7 N8 C16 179.6(3) . . . . ? Ru1 N7 N8 C16 1.8(4) . . . . ? Ru1 N1 C1 C2 -177.4(3) . . . . ? Ru1 N1 C1 C6 5.9(4) . . . . ? N1 C1 C2 C3 -177.2(4) . . . . ? C6 C1 C2 C3 -0.6(6) . . . . ? C1 C2 C3 C4 1.1(7) . . . . ? C2 C3 C4 C5 -0.6(7) . . . . ? C3 C4 C5 C6 -0.4(6) . . . . ? Ru1 N2 C6 C5 178.6(3) . . . . ? Ru1 N2 C6 C1 -3.2(4) . . . . ? C4 C5 C6 N2 179.0(4) . . . . ? C4 C5 C6 C1 0.8(6) . . . . ? N1 C1 C6 N2 -1.7(5) . . . . ? C2 C1 C6 N2 -178.8(4) . . . . ? N1 C1 C6 C5 176.7(4) . . . . ? C2 C1 C6 C5 -0.4(6) . . . . ? N4 N3 C7 C8 1.2(5) . . . . ? Ru1 N3 C7 C8 -171.3(3) . . . . ? N3 C7 C8 C9 0.0(6) . . . . ? N3 N4 C9 C8 2.1(5) . . . . ? C16 N4 C9 C8 166.6(4) . . . . ? C7 C8 C9 N4 -1.2(5) . . . . ? N6 N5 C10 C11 -1.9(5) . . . . ? Ru1 N5 C10 C11 171.1(3) . . . . ? N5 C10 C11 C12 0.9(5) . . . . ? N5 N6 C12 C11 -1.6(5) . . . . ? C16 N6 C12 C11 -170.2(4) . . . . ? C10 C11 C12 N6 0.4(5) . . . . ? N8 N7 C13 C14 0.5(4) . . . . ? Ru1 N7 C13 C14 177.6(3) . . . . ? N7 C13 C14 C15 -1.0(5) . . . . ? N7 N8 C15 C14 -0.8(5) . . . . ? C16 N8 C15 C14 179.9(4) . . . . ? C13 C14 C15 N8 1.1(5) . . . . ? C15 N8 C16 N6 117.8(4) . . . . ? N7 N8 C16 N6 -61.5(5) . . . . ? C15 N8 C16 N4 -120.2(4) . . . . ? N7 N8 C16 N4 60.5(4) . . . . ? C12 N6 C16 N8 -129.9(4) . . . . ? N5 N6 C16 N8 62.3(5) . . . . ? C12 N6 C16 N4 107.6(5) . . . . ? N5 N6 C16 N4 -60.3(5) . . . . ? C9 N4 C16 N8 131.4(4) . . . . ? N3 N4 C16 N8 -65.0(4) . . . . ? C9 N4 C16 N6 -106.6(5) . . . . ? N3 N4 C16 N6 57.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.533 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.109 data_[2](ClO4)2 _database_code_depnum_ccdc_archive 'CCDC 904798' #TrackingRef '[2](ClO4)2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H38 Cl4 N16 O19 Ru2' _chemical_formula_weight 1294.72 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 '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 15.2839(6) _cell_length_b 16.3749(8) _cell_length_c 18.4186(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.073(4) _cell_angle_gamma 90.00 _cell_volume 4609.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10592 _cell_measurement_theta_min 3.3115 _cell_measurement_theta_max 32.5342 _exptl_crystal_description thin-plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2600 _exptl_absorpt_coefficient_mu 0.982 _exptl_absorpt_correction_T_min 0.7376 _exptl_absorpt_correction_T_max 0.8057 _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 39749 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.1009 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _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 8103 _reflns_number_gt 5218 _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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8103 _refine_ls_number_parameters 683 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.912 _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 0.65962(3) 0.52182(3) 0.28473(2) 0.01881(12) Uani 1 1 d . . . Ru2 Ru 0.84956(3) 0.11912(3) 0.32501(2) 0.01776(12) Uani 1 1 d . . . O1 O 0.7129(2) 0.6047(2) 0.20755(19) 0.0272(9) Uani 1 1 d . . . H1A H 0.6910 0.6545 0.2140 0.041 Uiso 1 1 d R . . H1B H 0.7002 0.5886 0.1626 0.041 Uiso 1 1 d R . . O2 O 0.7947(2) 0.0285(2) 0.25746(19) 0.0271(9) Uani 1 1 d . . . H2A H 0.8203 -0.0196 0.2649 0.041 Uiso 1 1 d R . . H2B H 0.8013 0.0417 0.2108 0.041 Uiso 1 1 d R . . N1 N 0.7629(3) 0.5399(3) 0.3486(3) 0.0212(11) Uani 1 1 d . . . N2 N 0.7421(3) 0.4382(3) 0.2495(2) 0.0199(10) Uani 1 1 d D . . N3 N 0.5583(3) 0.4897(3) 0.2158(2) 0.0200(11) Uani 1 1 d . . . N4 N 0.4750(3) 0.4894(3) 0.2424(2) 0.0199(11) Uani 1 1 d . . . N5 N 0.5998(3) 0.4469(3) 0.3561(2) 0.0176(10) Uani 1 1 d . . . N6 N 0.5103(3) 0.4503(3) 0.3632(2) 0.0229(11) Uani 1 1 d . . . N7 N 0.5772(3) 0.6103(3) 0.3281(2) 0.0206(11) Uani 1 1 d . . . N8 N 0.4900(3) 0.5900(3) 0.3354(2) 0.0196(11) Uani 1 1 d . . . N9 N 0.7573(3) 0.1940(3) 0.2854(2) 0.0196(10) Uani 1 1 d . . . H9N H 0.7687 0.2291 0.2506 0.024 Uiso 1 1 calc R . . N10 N 0.7512(3) 0.1026(3) 0.3942(3) 0.0223(11) Uani 1 1 d . . . N11 N 0.9376(3) 0.0360(3) 0.3689(2) 0.0203(10) Uani 1 1 d . . . N12 N 1.0237(3) 0.0587(3) 0.3727(2) 0.0200(10) Uani 1 1 d . . . N13 N 0.9109(2) 0.2030(3) 0.3880(2) 0.0166(10) Uani 1 1 d . . . N14 N 1.0007(3) 0.2001(3) 0.3932(2) 0.0193(10) Uani 1 1 d . . . N15 N 0.9469(3) 0.1476(3) 0.2499(2) 0.0201(11) Uani 1 1 d . . . N16 N 1.0307(3) 0.1525(3) 0.2746(2) 0.0197(11) Uani 1 1 d . . . C1 C 0.8342(3) 0.4979(3) 0.3340(3) 0.0222(13) Uani 1 1 d . . . C2 C 0.9173(3) 0.5023(4) 0.3699(3) 0.0285(15) Uani 1 1 d . . . H2 H 0.9261 0.5382 0.4098 0.034 Uiso 1 1 calc R . . C3 C 0.9829(4) 0.4541(4) 0.3456(3) 0.0335(16) Uani 1 1 d . . . H3 H 1.0390 0.4587 0.3676 0.040 Uiso 1 1 calc R . . C4 C 0.9712(4) 0.3969(4) 0.2885(3) 0.0317(15) Uani 1 1 d . . . H4 H 1.0191 0.3637 0.2741 0.038 Uiso 1 1 calc R . . C5 C 0.8937(3) 0.3886(4) 0.2541(3) 0.0259(14) Uani 1 1 d . . . H5 H 0.8868 0.3498 0.2162 0.031 Uiso 1 1 calc R . . C6 C 0.8223(3) 0.4391(4) 0.2755(3) 0.0222(13) Uani 1 1 d . . . C7 C 0.5519(3) 0.4584(3) 0.1494(3) 0.0226(13) Uani 1 1 d . . . H7 H 0.5997 0.4508 0.1171 0.027 Uiso 1 1 calc R . . C8 C 0.4651(3) 0.4382(4) 0.1335(3) 0.0267(14) Uani 1 1 d . . . H8 H 0.4433 0.4161 0.0894 0.032 Uiso 1 1 calc R . . C9 C 0.4184(3) 0.4567(3) 0.1939(3) 0.0233(13) Uani 1 1 d . . . H9 H 0.3575 0.4482 0.2008 0.028 Uiso 1 1 calc R . . C10 C 0.6256(4) 0.3933(3) 0.4050(3) 0.0234(13) Uani 1 1 d . . . H10 H 0.6847 0.3778 0.4131 0.028 Uiso 1 1 calc R . . C11 C 0.5545(4) 0.3625(4) 0.4433(3) 0.0270(14) Uani 1 1 d . . . H11 H 0.5561 0.3230 0.4810 0.032 Uiso 1 1 calc R . . C12 C 0.4825(4) 0.3999(3) 0.4161(3) 0.0252(14) Uani 1 1 d . . . H12 H 0.4237 0.3921 0.4314 0.030 Uiso 1 1 calc R . . C13 C 0.5836(4) 0.6842(4) 0.3566(3) 0.0258(14) Uani 1 1 d . . . H13 H 0.6364 0.7146 0.3597 0.031 Uiso 1 1 calc R . . C14 C 0.5025(3) 0.7119(4) 0.3818(3) 0.0252(14) Uani 1 1 d . . . H14 H 0.4903 0.7630 0.4039 0.030 Uiso 1 1 calc R . . C15 C 0.4453(4) 0.6509(4) 0.3680(3) 0.0263(14) Uani 1 1 d . . . H15 H 0.3846 0.6509 0.3792 0.032 Uiso 1 1 calc R . . C16 C 0.4628(3) 0.5077(3) 0.3189(3) 0.0214(13) Uani 1 1 d . . . H16 H 0.3991 0.5026 0.3304 0.026 Uiso 1 1 calc R . . C17 C 0.6789(3) 0.1878(3) 0.3143(3) 0.0197(13) Uani 1 1 d . . . C18 C 0.6006(3) 0.2268(4) 0.2903(3) 0.0253(14) Uani 1 1 d . . . H18 H 0.6017 0.2618 0.2492 0.030 Uiso 1 1 calc R . . C19 C 0.5250(4) 0.2138(4) 0.3264(3) 0.0298(15) Uani 1 1 d . . . H19 H 0.4725 0.2384 0.3097 0.036 Uiso 1 1 calc R . . C20 C 0.5236(4) 0.1626(4) 0.3901(3) 0.0326(16) Uani 1 1 d . . . H20 H 0.4698 0.1550 0.4149 0.039 Uiso 1 1 calc R . . C21 C 0.5952(3) 0.1255(4) 0.4154(3) 0.0269(14) Uani 1 1 d . . . H21 H 0.5923 0.0930 0.4581 0.032 Uiso 1 1 calc R . . C22 C 0.6764(3) 0.1353(3) 0.3775(3) 0.0208(13) Uani 1 1 d . . . C23 C 0.9355(4) -0.0385(4) 0.3963(3) 0.0257(14) Uani 1 1 d . . . H23 H 0.8839 -0.0704 0.4008 0.031 Uiso 1 1 calc R . . C24 C 1.0182(4) -0.0647(4) 0.4179(3) 0.0290(14) Uani 1 1 d . . . H24 H 1.0333 -0.1158 0.4390 0.035 Uiso 1 1 calc R . . C25 C 1.0730(4) -0.0013(4) 0.4023(3) 0.0251(14) Uani 1 1 d . . . H25 H 1.1343 0.0004 0.4106 0.030 Uiso 1 1 calc R . . C26 C 0.8863(3) 0.2630(4) 0.4311(3) 0.0225(13) Uani 1 1 d . . . H26 H 0.8274 0.2794 0.4387 0.027 Uiso 1 1 calc R . . C27 C 0.9593(3) 0.2990(4) 0.4642(3) 0.0249(13) Uani 1 1 d . . . H27 H 0.9590 0.3431 0.4977 0.030 Uiso 1 1 calc R . . C28 C 1.0303(4) 0.2586(4) 0.4390(3) 0.0227(13) Uani 1 1 d . . . H28 H 1.0896 0.2692 0.4511 0.027 Uiso 1 1 calc R . . C29 C 0.9487(3) 0.1741(3) 0.1818(3) 0.0212(13) Uani 1 1 d . . . H29 H 0.8994 0.1767 0.1504 0.025 Uiso 1 1 calc R . . C30 C 1.0336(4) 0.1978(4) 0.1629(3) 0.0253(14) Uani 1 1 d . . . H30 H 1.0526 0.2189 0.1175 0.030 Uiso 1 1 calc R . . C31 C 1.0829(3) 0.1842(4) 0.2226(3) 0.0228(13) Uani 1 1 d . . . H31 H 1.1437 0.1950 0.2273 0.027 Uiso 1 1 calc R . . C32 C 1.0484(3) 0.1405(3) 0.3508(3) 0.0199(13) Uani 1 1 d . . . H32 H 1.1125 0.1480 0.3596 0.024 Uiso 1 1 calc R . . O10 O 0.7058(3) 0.2030(2) 0.65220(19) 0.0328(10) Uani 1 1 d . . . O11 O 0.8094(2) 0.6433(3) 0.0256(2) 0.0420(12) Uani 1 1 d . . . O12 O 0.7359(3) 0.1047(2) 0.56391(19) 0.0314(10) Uani 1 1 d . . . O13 O 0.8331(2) 0.2122(3) 0.5827(2) 0.0367(11) Uani 1 1 d . . . O14 O 0.6834(2) 0.0074(3) 0.0410(2) 0.0426(12) Uani 1 1 d . . . O15 O 0.7610(3) 0.0844(3) 0.1251(2) 0.0486(13) Uani 1 1 d . . . O16 O 0.8259(3) -0.0311(3) 0.0731(2) 0.0486(12) Uani 1 1 d . . . O17 O 0.8023(3) 0.0849(3) 0.0021(2) 0.0484(13) Uani 1 1 d . . . O22 O 0.7253(3) 0.5707(3) -0.0579(2) 0.0442(12) Uani 1 1 d . . . O33 O 0.6781(3) 0.5814(3) 0.0612(2) 0.0504(13) Uani 1 1 d . . . O44 O 0.6750(3) 0.6956(3) -0.0131(2) 0.0447(12) Uani 1 1 d . . . O55 O 0.6927(3) 0.8829(3) 0.1743(2) 0.0434(11) Uani 1 1 d . . . O66 O 0.8118(3) 0.8629(3) 0.2517(3) 0.0586(14) Uani 1 1 d . . . O77 O 0.7951(3) 0.7802(3) 0.1480(2) 0.0560(14) Uani 1 1 d . . . O88 O 0.7016(3) 0.7647(3) 0.2450(2) 0.0502(13) Uani 1 1 d . . . O99 O 0.6966(2) 0.2382(3) 0.52932(19) 0.0315(10) Uani 1 1 d . . . O101 O 0.7926(3) -0.1596(3) -0.0313(2) 0.0432(12) Uani 1 1 d GD . . Cl1 Cl 0.72275(8) 0.62348(9) 0.00353(7) 0.0263(3) Uani 1 1 d . . . Cl2 Cl 0.75014(9) 0.82306(9) 0.20295(8) 0.0299(3) Uani 1 1 d . . . Cl3 Cl 0.74327(8) 0.19022(9) 0.58104(7) 0.0215(3) Uani 1 1 d . . . Cl4 Cl 0.76826(9) 0.03631(10) 0.05932(8) 0.0313(4) Uani 1 1 d . . . H1N H 0.766(3) 0.568(3) 0.384(3) 0.013(16) Uiso 1 1 d . . . H2N H 0.730(3) 0.399(3) 0.211(2) 0.028(16) Uiso 1 1 d D . . H10N H 0.757(4) 0.076(5) 0.434(4) 0.06(2) Uiso 1 1 d . . . H102 H 0.790(3) -0.123(3) 0.011(2) 0.032(17) Uiso 1 1 d D . . H101 H 0.750(3) -0.204(3) -0.022(3) 0.06(2) Uiso 1 1 d 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 0.0148(2) 0.0200(3) 0.0216(2) -0.0017(2) -0.00130(17) 0.0000(2) Ru2 0.0147(2) 0.0204(3) 0.0181(2) -0.0009(2) -0.00020(17) 0.0003(2) O1 0.024(2) 0.024(3) 0.034(2) 0.0001(18) 0.0006(17) -0.0033(18) O2 0.031(2) 0.023(2) 0.027(2) -0.0017(18) -0.0010(17) -0.0002(19) N1 0.024(3) 0.016(3) 0.024(3) -0.005(2) -0.003(2) -0.002(2) N2 0.018(2) 0.023(3) 0.019(2) -0.003(2) -0.0035(19) -0.004(2) N3 0.014(2) 0.025(3) 0.021(2) 0.002(2) -0.0015(18) -0.002(2) N4 0.013(2) 0.022(3) 0.024(3) -0.002(2) 0.0010(19) -0.002(2) N5 0.013(2) 0.015(3) 0.025(2) -0.005(2) -0.0026(19) 0.0035(19) N6 0.021(2) 0.024(3) 0.024(3) 0.000(2) 0.000(2) 0.002(2) N7 0.015(2) 0.021(3) 0.026(3) -0.001(2) 0.0009(19) -0.006(2) N8 0.014(2) 0.021(3) 0.024(3) 0.001(2) 0.0018(19) 0.002(2) N9 0.021(2) 0.018(3) 0.020(2) -0.003(2) 0.0023(19) 0.000(2) N10 0.027(3) 0.022(3) 0.018(3) -0.001(2) 0.000(2) -0.004(2) N11 0.024(2) 0.016(3) 0.021(2) -0.002(2) 0.0029(19) 0.000(2) N12 0.017(2) 0.018(3) 0.025(3) 0.001(2) -0.0016(19) 0.002(2) N13 0.008(2) 0.018(3) 0.024(3) 0.003(2) -0.0005(18) 0.0017(19) N14 0.015(2) 0.023(3) 0.020(2) 0.000(2) -0.0016(19) 0.002(2) N15 0.012(2) 0.025(3) 0.023(3) -0.001(2) -0.0007(19) 0.002(2) N16 0.020(2) 0.022(3) 0.018(2) 0.000(2) 0.0000(19) 0.005(2) C1 0.021(3) 0.026(4) 0.020(3) 0.006(3) -0.001(2) -0.007(3) C2 0.024(3) 0.030(4) 0.032(3) 0.008(3) -0.004(3) -0.008(3) C3 0.020(3) 0.038(4) 0.042(4) 0.012(3) -0.005(3) -0.006(3) C4 0.019(3) 0.031(4) 0.046(4) 0.011(3) 0.005(3) 0.006(3) C5 0.025(3) 0.023(4) 0.029(3) 0.007(3) 0.006(2) 0.007(3) C6 0.017(3) 0.025(4) 0.025(3) 0.008(3) 0.003(2) -0.002(3) C7 0.022(3) 0.020(4) 0.026(3) 0.000(3) -0.001(2) 0.003(3) C8 0.027(3) 0.028(4) 0.025(3) -0.006(3) -0.007(3) 0.001(3) C9 0.015(3) 0.022(4) 0.032(3) 0.005(3) -0.008(2) -0.003(2) C10 0.028(3) 0.026(4) 0.017(3) -0.004(3) -0.007(2) 0.001(3) C11 0.034(3) 0.028(4) 0.020(3) 0.001(3) -0.003(3) 0.001(3) C12 0.028(3) 0.026(4) 0.021(3) 0.001(3) 0.008(3) -0.002(3) C13 0.032(3) 0.025(4) 0.020(3) 0.001(3) -0.004(3) -0.005(3) C14 0.027(3) 0.023(4) 0.025(3) -0.001(3) 0.006(3) 0.000(3) C15 0.025(3) 0.031(4) 0.023(3) 0.005(3) 0.003(2) 0.004(3) C16 0.017(3) 0.020(4) 0.028(3) 0.003(3) 0.000(2) -0.003(2) C17 0.023(3) 0.016(3) 0.020(3) -0.008(2) -0.001(2) 0.005(2) C18 0.025(3) 0.029(4) 0.022(3) -0.003(3) -0.003(2) 0.002(3) C19 0.023(3) 0.037(4) 0.029(3) -0.005(3) -0.003(3) 0.001(3) C20 0.015(3) 0.045(4) 0.038(4) -0.016(3) 0.006(3) -0.007(3) C21 0.021(3) 0.036(4) 0.024(3) 0.000(3) 0.004(2) -0.005(3) C22 0.020(3) 0.026(4) 0.017(3) -0.005(2) 0.000(2) -0.005(3) C23 0.034(3) 0.021(4) 0.022(3) 0.000(3) 0.006(3) 0.004(3) C24 0.040(4) 0.023(4) 0.024(3) 0.005(3) 0.000(3) 0.013(3) C25 0.026(3) 0.032(4) 0.017(3) -0.003(3) 0.002(2) 0.013(3) C26 0.016(3) 0.030(4) 0.021(3) 0.000(3) 0.003(2) -0.001(3) C27 0.029(3) 0.023(4) 0.023(3) -0.003(3) 0.004(3) 0.001(3) C28 0.022(3) 0.032(4) 0.015(3) -0.003(3) -0.003(2) -0.007(3) C29 0.026(3) 0.020(3) 0.018(3) -0.001(2) 0.000(2) 0.005(3) C30 0.030(3) 0.024(4) 0.022(3) 0.002(3) 0.004(3) 0.000(3) C31 0.019(3) 0.026(4) 0.024(3) -0.007(3) 0.006(2) -0.006(3) C32 0.011(3) 0.027(4) 0.022(3) -0.002(2) 0.000(2) -0.001(2) O10 0.049(3) 0.030(3) 0.019(2) 0.0023(18) 0.0081(19) 0.003(2) O11 0.024(2) 0.048(3) 0.054(3) -0.012(2) -0.013(2) -0.003(2) O12 0.045(3) 0.019(3) 0.031(2) -0.0057(18) 0.0035(19) -0.0015(19) O13 0.025(2) 0.045(3) 0.041(3) 0.005(2) -0.0054(19) -0.004(2) O14 0.020(2) 0.051(3) 0.057(3) 0.016(2) -0.0098(19) -0.012(2) O15 0.062(3) 0.058(3) 0.026(2) -0.010(2) -0.008(2) 0.013(3) O16 0.039(3) 0.045(3) 0.062(3) -0.002(2) -0.017(2) 0.019(2) O17 0.041(3) 0.062(4) 0.042(3) 0.015(2) 0.009(2) -0.010(2) O22 0.033(2) 0.062(3) 0.038(3) -0.021(2) -0.0056(19) 0.000(2) O33 0.063(3) 0.046(3) 0.042(3) 0.009(2) 0.013(2) -0.006(3) O44 0.041(3) 0.027(3) 0.066(3) 0.008(2) -0.010(2) 0.010(2) O55 0.040(3) 0.035(3) 0.055(3) 0.007(2) -0.013(2) 0.014(2) O66 0.044(3) 0.030(3) 0.102(4) -0.005(3) -0.040(3) 0.002(2) O77 0.073(3) 0.043(3) 0.052(3) 0.002(2) 0.040(3) 0.013(3) O88 0.053(3) 0.037(3) 0.061(3) 0.008(2) 0.026(2) -0.009(2) O99 0.031(2) 0.036(3) 0.028(2) 0.0075(19) -0.0102(17) 0.004(2) O101 0.059(3) 0.032(3) 0.039(3) 0.006(2) -0.007(2) -0.004(2) Cl1 0.0223(7) 0.0288(9) 0.0279(8) -0.0025(7) -0.0024(6) 0.0017(7) Cl2 0.0265(8) 0.0249(9) 0.0383(9) 0.0027(7) 0.0051(6) 0.0017(7) Cl3 0.0228(7) 0.0227(8) 0.0191(7) 0.0006(6) -0.0010(6) 0.0014(6) Cl4 0.0246(8) 0.0385(11) 0.0307(8) 0.0020(7) -0.0040(6) -0.0025(7) _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 1.972(4) . ? Ru1 N1 1.990(5) . ? Ru1 N5 2.017(4) . ? Ru1 N3 2.068(4) . ? Ru1 N7 2.080(4) . ? Ru1 O1 2.128(3) . ? Ru2 N10 1.990(4) . ? Ru2 N9 2.004(4) . ? Ru2 N13 2.028(4) . ? Ru2 N11 2.077(4) . ? Ru2 N15 2.086(4) . ? Ru2 O2 2.109(4) . ? O1 H1A 0.8895 . ? O1 H1B 0.8896 . ? O2 H2A 0.8907 . ? O2 H2B 0.8912 . ? N1 C1 1.316(7) . ? N1 H1N 0.80(5) . ? N2 C6 1.315(6) . ? N2 H2N 0.98(2) . ? N3 C7 1.331(6) . ? N3 N4 1.366(5) . ? N4 C9 1.354(7) . ? N4 C16 1.452(6) . ? N5 C10 1.318(7) . ? N5 N6 1.376(5) . ? N6 C12 1.347(6) . ? N6 C16 1.440(7) . ? N7 C13 1.322(7) . ? N7 N8 1.380(5) . ? N8 C15 1.351(7) . ? N8 C16 1.443(7) . ? N9 C17 1.316(6) . ? N9 H9N 0.8800 . ? N10 C22 1.299(7) . ? N10 H10N 0.85(7) . ? N11 C23 1.321(7) . ? N11 N12 1.370(6) . ? N12 C25 1.352(7) . ? N12 C32 1.448(7) . ? N13 C26 1.317(6) . ? N13 N14 1.376(5) . ? N14 C28 1.353(7) . ? N14 C32 1.448(6) . ? N15 C29 1.327(6) . ? N15 N16 1.361(6) . ? N16 C31 1.349(6) . ? N16 C32 1.443(6) . ? C1 C2 1.434(7) . ? C1 C6 1.456(8) . ? C2 C3 1.353(8) . ? C2 H2 0.9500 . ? C3 C4 1.420(8) . ? C3 H3 0.9500 . ? C4 C5 1.349(8) . ? C4 H4 0.9500 . ? C5 C6 1.424(7) . ? C5 H5 0.9500 . ? C7 C8 1.397(7) . ? C7 H7 0.9500 . ? C8 C9 1.357(7) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.391(7) . ? C10 H10 0.9500 . ? C11 C12 1.355(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.399(7) . ? C13 H13 0.9500 . ? C14 C15 1.351(8) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16 1.0000 . ? C17 C18 1.427(7) . ? C17 C22 1.448(7) . ? C18 C19 1.351(7) . ? C18 H18 0.9500 . ? C19 C20 1.442(8) . ? C19 H19 0.9500 . ? C20 C21 1.335(8) . ? C20 H20 0.9500 . ? C21 C22 1.434(7) . ? C21 H21 0.9500 . ? C23 C24 1.393(8) . ? C23 H23 0.9500 . ? C24 C25 1.365(8) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.400(7) . ? C26 H26 0.9500 . ? C27 C28 1.354(7) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.399(7) . ? C29 H29 0.9500 . ? C30 C31 1.351(7) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 H32 1.0000 . ? O10 Cl3 1.446(4) . ? O11 Cl1 1.422(4) . ? O12 Cl3 1.439(4) . ? O13 Cl3 1.420(4) . ? O14 Cl4 1.421(4) . ? O15 Cl4 1.449(4) . ? O16 Cl4 1.434(4) . ? O17 Cl4 1.420(4) . ? O22 Cl1 1.425(4) . ? O33 Cl1 1.440(4) . ? O44 Cl1 1.421(4) . ? O55 Cl2 1.417(4) . ? O66 Cl2 1.455(5) . ? O77 Cl2 1.411(4) . ? O88 Cl2 1.437(4) . ? O99 Cl3 1.426(4) . ? O101 H102 0.98(2) . ? O101 H101 1.00(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 N2 Ru1 N1 77.90(19) . . ? N2 Ru1 N5 94.76(17) . . ? N1 Ru1 N5 93.71(18) . . ? N2 Ru1 N3 95.76(17) . . ? N1 Ru1 N3 173.31(19) . . ? N5 Ru1 N3 84.61(17) . . ? N2 Ru1 N7 176.30(17) . . ? N1 Ru1 N7 98.61(18) . . ? N5 Ru1 N7 84.17(16) . . ? N3 Ru1 N7 87.68(17) . . ? N2 Ru1 O1 88.70(16) . . ? N1 Ru1 O1 89.78(17) . . ? N5 Ru1 O1 175.53(15) . . ? N3 Ru1 O1 92.24(15) . . ? N7 Ru1 O1 92.55(15) . . ? N10 Ru2 N9 77.57(19) . . ? N10 Ru2 N13 94.28(17) . . ? N9 Ru2 N13 96.79(17) . . ? N10 Ru2 N11 98.68(19) . . ? N9 Ru2 N11 175.70(17) . . ? N13 Ru2 N11 85.53(17) . . ? N10 Ru2 N15 174.3(2) . . ? N9 Ru2 N15 97.11(17) . . ? N13 Ru2 N15 84.19(16) . . ? N11 Ru2 N15 86.71(16) . . ? N10 Ru2 O2 88.96(16) . . ? N9 Ru2 O2 86.36(16) . . ? N13 Ru2 O2 175.90(15) . . ? N11 Ru2 O2 91.49(16) . . ? N15 Ru2 O2 92.83(15) . . ? Ru1 O1 H1A 110.5 . . ? Ru1 O1 H1B 110.4 . . ? H1A O1 H1B 108.3 . . ? Ru2 O2 H2A 110.9 . . ? Ru2 O2 H2B 110.6 . . ? H2A O2 H2B 108.2 . . ? C1 N1 Ru1 117.2(4) . . ? C1 N1 H1N 115(4) . . ? Ru1 N1 H1N 127(4) . . ? C6 N2 Ru1 118.0(4) . . ? C6 N2 H2N 116(3) . . ? Ru1 N2 H2N 126(3) . . ? C7 N3 N4 105.1(4) . . ? C7 N3 Ru1 135.8(3) . . ? N4 N3 Ru1 118.6(3) . . ? C9 N4 N3 111.1(4) . . ? C9 N4 C16 129.8(4) . . ? N3 N4 C16 117.9(4) . . ? C10 N5 N6 105.0(4) . . ? C10 N5 Ru1 135.7(4) . . ? N6 N5 Ru1 119.3(3) . . ? C12 N6 N5 111.0(4) . . ? C12 N6 C16 130.6(4) . . ? N5 N6 C16 118.3(4) . . ? C13 N7 N8 104.6(4) . . ? C13 N7 Ru1 138.2(4) . . ? N8 N7 Ru1 117.0(3) . . ? C15 N8 N7 110.8(4) . . ? C15 N8 C16 129.6(4) . . ? N7 N8 C16 118.9(4) . . ? C17 N9 Ru2 116.5(4) . . ? C17 N9 H9N 121.7 . . ? Ru2 N9 H9N 121.7 . . ? C22 N10 Ru2 117.3(4) . . ? C22 N10 H10N 120(5) . . ? Ru2 N10 H10N 122(5) . . ? C23 N11 N12 104.8(4) . . ? C23 N11 Ru2 137.6(4) . . ? N12 N11 Ru2 117.7(3) . . ? C25 N12 N11 110.9(4) . . ? C25 N12 C32 129.7(4) . . ? N11 N12 C32 119.2(4) . . ? C26 N13 N14 105.6(4) . . ? C26 N13 Ru2 135.9(3) . . ? N14 N13 Ru2 118.4(3) . . ? C28 N14 N13 110.5(4) . . ? C28 N14 C32 130.2(4) . . ? N13 N14 C32 119.3(4) . . ? C29 N15 N16 106.0(4) . . ? C29 N15 Ru2 135.7(4) . . ? N16 N15 Ru2 117.6(3) . . ? C31 N16 N15 110.0(4) . . ? C31 N16 C32 129.2(4) . . ? N15 N16 C32 119.5(4) . . ? N1 C1 C2 127.7(5) . . ? N1 C1 C6 113.2(5) . . ? C2 C1 C6 119.0(5) . . ? C3 C2 C1 118.3(6) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 122.5(6) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C5 C4 C3 121.6(5) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 118.9(6) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? N2 C6 C5 127.3(5) . . ? N2 C6 C1 113.0(5) . . ? C5 C6 C1 119.6(5) . . ? N3 C7 C8 110.7(5) . . ? N3 C7 H7 124.7 . . ? C8 C7 H7 124.7 . . ? C9 C8 C7 106.0(5) . . ? C9 C8 H8 127.0 . . ? C7 C8 H8 127.0 . . ? N4 C9 C8 107.1(5) . . ? N4 C9 H9 126.5 . . ? C8 C9 H9 126.5 . . ? N5 C10 C11 110.8(5) . . ? N5 C10 H10 124.6 . . ? C11 C10 H10 124.6 . . ? C12 C11 C10 106.5(5) . . ? C12 C11 H11 126.8 . . ? C10 C11 H11 126.8 . . ? N6 C12 C11 106.7(5) . . ? N6 C12 H12 126.6 . . ? C11 C12 H12 126.6 . . ? N7 C13 C14 111.3(5) . . ? N7 C13 H13 124.3 . . ? C14 C13 H13 124.3 . . ? C15 C14 C13 105.8(5) . . ? C15 C14 H14 127.1 . . ? C13 C14 H14 127.1 . . ? N8 C15 C14 107.5(5) . . ? N8 C15 H15 126.3 . . ? C14 C15 H15 126.3 . . ? N6 C16 N8 110.1(4) . . ? N6 C16 N4 110.5(4) . . ? N8 C16 N4 111.1(4) . . ? N6 C16 H16 108.4 . . ? N8 C16 H16 108.4 . . ? N4 C16 H16 108.4 . . ? N9 C17 C18 127.2(5) . . ? N9 C17 C22 113.3(5) . . ? C18 C17 C22 119.5(5) . . ? C19 C18 C17 119.6(5) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 120.4(5) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 122.4(5) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C20 C21 C22 119.2(5) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? N10 C22 C21 127.0(5) . . ? N10 C22 C17 114.2(5) . . ? C21 C22 C17 118.8(5) . . ? N11 C23 C24 111.8(5) . . ? N11 C23 H23 124.1 . . ? C24 C23 H23 124.1 . . ? C25 C24 C23 105.1(5) . . ? C25 C24 H24 127.4 . . ? C23 C24 H24 127.4 . . ? N12 C25 C24 107.3(5) . . ? N12 C25 H25 126.3 . . ? C24 C25 H25 126.3 . . ? N13 C26 C27 110.4(5) . . ? N13 C26 H26 124.8 . . ? C27 C26 H26 124.8 . . ? C28 C27 C26 106.4(5) . . ? C28 C27 H27 126.8 . . ? C26 C27 H27 126.8 . . ? N14 C28 C27 107.0(5) . . ? N14 C28 H28 126.5 . . ? C27 C28 H28 126.5 . . ? N15 C29 C30 110.3(5) . . ? N15 C29 H29 124.9 . . ? C30 C29 H29 124.9 . . ? C31 C30 C29 105.5(5) . . ? C31 C30 H30 127.2 . . ? C29 C30 H30 127.2 . . ? N16 C31 C30 108.1(5) . . ? N16 C31 H31 125.9 . . ? C30 C31 H31 125.9 . . ? N16 C32 N12 110.4(4) . . ? N16 C32 N14 109.8(4) . . ? N12 C32 N14 110.0(4) . . ? N16 C32 H32 108.9 . . ? N12 C32 H32 108.9 . . ? N14 C32 H32 108.9 . . ? H102 O101 H101 107(5) . . ? O44 Cl1 O11 110.4(3) . . ? O44 Cl1 O22 110.3(3) . . ? O11 Cl1 O22 109.8(2) . . ? O44 Cl1 O33 108.2(3) . . ? O11 Cl1 O33 109.9(3) . . ? O22 Cl1 O33 108.1(3) . . ? O77 Cl2 O55 112.2(3) . . ? O77 Cl2 O88 108.0(3) . . ? O55 Cl2 O88 109.9(3) . . ? O77 Cl2 O66 110.5(3) . . ? O55 Cl2 O66 108.7(3) . . ? O88 Cl2 O66 107.5(3) . . ? O13 Cl3 O99 111.0(2) . . ? O13 Cl3 O12 109.1(3) . . ? O99 Cl3 O12 110.5(2) . . ? O13 Cl3 O10 109.1(2) . . ? O99 Cl3 O10 109.1(2) . . ? O12 Cl3 O10 107.9(2) . . ? O17 Cl4 O14 110.3(3) . . ? O17 Cl4 O16 109.7(3) . . ? O14 Cl4 O16 110.2(3) . . ? O17 Cl4 O15 110.1(3) . . ? O14 Cl4 O15 108.0(3) . . ? O16 Cl4 O15 108.5(3) . . ? 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 N1 C1 6.5(4) . . . . ? N5 Ru1 N1 C1 100.5(4) . . . . ? N3 Ru1 N1 C1 25.3(17) . . . . ? N7 Ru1 N1 C1 -174.8(4) . . . . ? O1 Ru1 N1 C1 -82.3(4) . . . . ? N1 Ru1 N2 C6 -7.2(4) . . . . ? N5 Ru1 N2 C6 -100.0(4) . . . . ? N3 Ru1 N2 C6 174.9(4) . . . . ? N7 Ru1 N2 C6 -27(3) . . . . ? O1 Ru1 N2 C6 82.8(4) . . . . ? N2 Ru1 N3 C7 -30.9(6) . . . . ? N1 Ru1 N3 C7 -49.3(17) . . . . ? N5 Ru1 N3 C7 -125.1(5) . . . . ? N7 Ru1 N3 C7 150.5(5) . . . . ? O1 Ru1 N3 C7 58.1(5) . . . . ? N2 Ru1 N3 N4 139.6(4) . . . . ? N1 Ru1 N3 N4 121.1(14) . . . . ? N5 Ru1 N3 N4 45.3(4) . . . . ? N7 Ru1 N3 N4 -39.1(4) . . . . ? O1 Ru1 N3 N4 -131.5(4) . . . . ? C7 N3 N4 C9 1.5(6) . . . . ? Ru1 N3 N4 C9 -171.6(4) . . . . ? C7 N3 N4 C16 170.0(5) . . . . ? Ru1 N3 N4 C16 -3.1(6) . . . . ? N2 Ru1 N5 C10 45.6(5) . . . . ? N1 Ru1 N5 C10 -32.5(5) . . . . ? N3 Ru1 N5 C10 141.0(5) . . . . ? N7 Ru1 N5 C10 -130.8(5) . . . . ? O1 Ru1 N5 C10 -173.8(18) . . . . ? N2 Ru1 N5 N6 -138.9(4) . . . . ? N1 Ru1 N5 N6 142.9(4) . . . . ? N3 Ru1 N5 N6 -43.6(4) . . . . ? N7 Ru1 N5 N6 44.6(4) . . . . ? O1 Ru1 N5 N6 2(2) . . . . ? C10 N5 N6 C12 0.5(6) . . . . ? Ru1 N5 N6 C12 -176.2(3) . . . . ? C10 N5 N6 C16 176.8(5) . . . . ? Ru1 N5 N6 C16 0.0(6) . . . . ? N2 Ru1 N7 C13 54(3) . . . . ? N1 Ru1 N7 C13 34.9(6) . . . . ? N5 Ru1 N7 C13 127.7(6) . . . . ? N3 Ru1 N7 C13 -147.4(5) . . . . ? O1 Ru1 N7 C13 -55.3(5) . . . . ? N2 Ru1 N7 N8 -120(3) . . . . ? N1 Ru1 N7 N8 -140.0(3) . . . . ? N5 Ru1 N7 N8 -47.1(3) . . . . ? N3 Ru1 N7 N8 37.7(3) . . . . ? O1 Ru1 N7 N8 129.8(3) . . . . ? C13 N7 N8 C15 -0.1(6) . . . . ? Ru1 N7 N8 C15 176.4(3) . . . . ? C13 N7 N8 C16 -171.2(4) . . . . ? Ru1 N7 N8 C16 5.2(5) . . . . ? N10 Ru2 N9 C17 -9.4(4) . . . . ? N13 Ru2 N9 C17 -102.3(4) . . . . ? N11 Ru2 N9 C17 20(2) . . . . ? N15 Ru2 N9 C17 172.8(4) . . . . ? O2 Ru2 N9 C17 80.4(4) . . . . ? N9 Ru2 N10 C22 8.9(4) . . . . ? N13 Ru2 N10 C22 104.9(4) . . . . ? N11 Ru2 N10 C22 -169.0(4) . . . . ? N15 Ru2 N10 C22 31(2) . . . . ? O2 Ru2 N10 C22 -77.6(4) . . . . ? N10 Ru2 N11 C23 41.4(5) . . . . ? N9 Ru2 N11 C23 12(2) . . . . ? N13 Ru2 N11 C23 135.1(5) . . . . ? N15 Ru2 N11 C23 -140.5(5) . . . . ? O2 Ru2 N11 C23 -47.8(5) . . . . ? N10 Ru2 N11 N12 -139.0(3) . . . . ? N9 Ru2 N11 N12 -168(2) . . . . ? N13 Ru2 N11 N12 -45.4(3) . . . . ? N15 Ru2 N11 N12 39.0(3) . . . . ? O2 Ru2 N11 N12 131.8(3) . . . . ? C23 N11 N12 C25 -0.3(5) . . . . ? Ru2 N11 N12 C25 -180.0(3) . . . . ? C23 N11 N12 C32 -176.2(4) . . . . ? Ru2 N11 N12 C32 4.1(5) . . . . ? N10 Ru2 N13 C26 -37.0(5) . . . . ? N9 Ru2 N13 C26 40.9(5) . . . . ? N11 Ru2 N13 C26 -135.4(5) . . . . ? N15 Ru2 N13 C26 137.4(5) . . . . ? O2 Ru2 N13 C26 -179(100) . . . . ? N10 Ru2 N13 N14 139.7(4) . . . . ? N9 Ru2 N13 N14 -142.3(3) . . . . ? N11 Ru2 N13 N14 41.3(3) . . . . ? N15 Ru2 N13 N14 -45.8(3) . . . . ? O2 Ru2 N13 N14 -2(2) . . . . ? C26 N13 N14 C28 -0.5(6) . . . . ? Ru2 N13 N14 C28 -178.1(3) . . . . ? C26 N13 N14 C32 -179.0(4) . . . . ? Ru2 N13 N14 C32 3.3(6) . . . . ? N10 Ru2 N15 C29 -49(2) . . . . ? N9 Ru2 N15 C29 -27.2(5) . . . . ? N13 Ru2 N15 C29 -123.3(5) . . . . ? N11 Ru2 N15 C29 150.9(5) . . . . ? O2 Ru2 N15 C29 59.5(5) . . . . ? N10 Ru2 N15 N16 120.2(18) . . . . ? N9 Ru2 N15 N16 141.6(4) . . . . ? N13 Ru2 N15 N16 45.4(4) . . . . ? N11 Ru2 N15 N16 -40.4(4) . . . . ? O2 Ru2 N15 N16 -131.7(4) . . . . ? C29 N15 N16 C31 1.9(6) . . . . ? Ru2 N15 N16 C31 -170.0(3) . . . . ? C29 N15 N16 C32 170.0(4) . . . . ? Ru2 N15 N16 C32 -1.8(6) . . . . ? Ru1 N1 C1 C2 177.4(4) . . . . ? Ru1 N1 C1 C6 -4.8(6) . . . . ? N1 C1 C2 C3 -179.3(6) . . . . ? C6 C1 C2 C3 3.1(8) . . . . ? C1 C2 C3 C4 -3.1(8) . . . . ? C2 C3 C4 C5 1.3(9) . . . . ? C3 C4 C5 C6 0.5(8) . . . . ? Ru1 N2 C6 C5 -175.2(4) . . . . ? Ru1 N2 C6 C1 6.7(6) . . . . ? C4 C5 C6 N2 -178.3(5) . . . . ? C4 C5 C6 C1 -0.3(8) . . . . ? N1 C1 C6 N2 -1.1(7) . . . . ? C2 C1 C6 N2 176.8(4) . . . . ? N1 C1 C6 C5 -179.4(5) . . . . ? C2 C1 C6 C5 -1.5(7) . . . . ? N4 N3 C7 C8 0.0(6) . . . . ? Ru1 N3 C7 C8 171.3(4) . . . . ? N3 C7 C8 C9 -1.4(7) . . . . ? N3 N4 C9 C8 -2.4(6) . . . . ? C16 N4 C9 C8 -169.2(5) . . . . ? C7 C8 C9 N4 2.3(6) . . . . ? N6 N5 C10 C11 -0.1(6) . . . . ? Ru1 N5 C10 C11 175.8(4) . . . . ? N5 C10 C11 C12 -0.4(7) . . . . ? N5 N6 C12 C11 -0.7(6) . . . . ? C16 N6 C12 C11 -176.4(5) . . . . ? C10 C11 C12 N6 0.6(6) . . . . ? N8 N7 C13 C14 -0.3(6) . . . . ? Ru1 N7 C13 C14 -175.6(4) . . . . ? N7 C13 C14 C15 0.6(6) . . . . ? N7 N8 C15 C14 0.5(6) . . . . ? C16 N8 C15 C14 170.4(5) . . . . ? C13 C14 C15 N8 -0.6(6) . . . . ? C12 N6 C16 N8 113.7(6) . . . . ? N5 N6 C16 N8 -61.7(6) . . . . ? C12 N6 C16 N4 -123.2(6) . . . . ? N5 N6 C16 N4 61.4(6) . . . . ? C15 N8 C16 N6 -111.6(6) . . . . ? N7 N8 C16 N6 57.7(5) . . . . ? C15 N8 C16 N4 125.7(5) . . . . ? N7 N8 C16 N4 -65.1(6) . . . . ? C9 N4 C16 N6 107.2(6) . . . . ? N3 N4 C16 N6 -58.9(6) . . . . ? C9 N4 C16 N8 -130.3(6) . . . . ? N3 N4 C16 N8 63.7(6) . . . . ? Ru2 N9 C17 C18 -172.2(5) . . . . ? Ru2 N9 C17 C22 8.4(6) . . . . ? N9 C17 C18 C19 180.0(5) . . . . ? C22 C17 C18 C19 -0.7(8) . . . . ? C17 C18 C19 C20 1.8(9) . . . . ? C18 C19 C20 C21 -0.9(9) . . . . ? C19 C20 C21 C22 -1.2(9) . . . . ? Ru2 N10 C22 C21 174.0(4) . . . . ? Ru2 N10 C22 C17 -7.1(6) . . . . ? C20 C21 C22 N10 -178.9(6) . . . . ? C20 C21 C22 C17 2.3(8) . . . . ? N9 C17 C22 N10 -1.0(7) . . . . ? C18 C17 C22 N10 179.6(5) . . . . ? N9 C17 C22 C21 178.0(5) . . . . ? C18 C17 C22 C21 -1.4(8) . . . . ? N12 N11 C23 C24 0.1(6) . . . . ? Ru2 N11 C23 C24 179.7(4) . . . . ? N11 C23 C24 C25 0.1(6) . . . . ? N11 N12 C25 C24 0.3(6) . . . . ? C32 N12 C25 C24 175.7(5) . . . . ? C23 C24 C25 N12 -0.3(6) . . . . ? N14 N13 C26 C27 0.1(6) . . . . ? Ru2 N13 C26 C27 177.1(4) . . . . ? N13 C26 C27 C28 0.3(6) . . . . ? N13 N14 C28 C27 0.7(6) . . . . ? C32 N14 C28 C27 179.1(5) . . . . ? C26 C27 C28 N14 -0.6(6) . . . . ? N16 N15 C29 C30 -1.2(6) . . . . ? Ru2 N15 C29 C30 168.5(4) . . . . ? N15 C29 C30 C31 0.1(6) . . . . ? N15 N16 C31 C30 -1.8(6) . . . . ? C32 N16 C31 C30 -168.5(5) . . . . ? C29 C30 C31 N16 1.1(6) . . . . ? C31 N16 C32 N12 -132.0(5) . . . . ? N15 N16 C32 N12 62.4(6) . . . . ? C31 N16 C32 N14 106.6(6) . . . . ? N15 N16 C32 N14 -59.0(6) . . . . ? C25 N12 C32 N16 121.1(5) . . . . ? N11 N12 C32 N16 -63.8(5) . . . . ? C25 N12 C32 N14 -117.5(5) . . . . ? N11 N12 C32 N14 57.5(6) . . . . ? C28 N14 C32 N16 -119.4(6) . . . . ? N13 N14 C32 N16 58.9(5) . . . . ? C28 N14 C32 N12 118.9(6) . . . . ? N13 N14 C32 N12 -62.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.220 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.133