# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Ochocki, Justyn' _publ_contact_author_email justynochocki@yahoo.com _publ_section_title ; Synthesis, single-crystal and solution structure analysis and in vitro cytotoxic activity of two novel complexes of ruthenium(II) with in situ formed flavanone-based ligands ; loop_ _publ_author_name L.Checinska A.Erxleben A.Garza-Ortiz M.Kasprzak J.Ochocki J.Reedijk L.Szmigiero E.Zyner # Attachment '- Ru_ethoxy.cif' data_Ru_ethoxy _database_code_depnum_ccdc_archive 'CCDC 779229' #TrackingRef '- Ru_ethoxy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H34 Cl2 N2 O8 Ru' _chemical_formula_weight 770.60 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 C2/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 22.482(4) _cell_length_b 9.126(2) _cell_length_c 18.052(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.55(3) _cell_angle_gamma 90.00 _cell_volume 3696.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3042 _cell_measurement_theta_min 4.61 _cell_measurement_theta_max 24.71 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8864 _exptl_absorpt_correction_T_max 0.9408 _exptl_absorpt_process_details Denzo,Scalepack,Otwinowski,Minor,1997 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3042 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.1260 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.61 _diffrn_reflns_theta_max 24.71 _reflns_number_total 3042 _reflns_number_gt 1354 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonis KappaCCD' _computing_cell_refinement Denzo,Scalepack,Otwinowski,Minor,1997 _computing_data_reduction Denzo,Scalepack,Otwinowski,Minor,1997 _computing_structure_solution SHELXS-97(Sheldrick,1990) _computing_structure_refinement SHELXL-97(Sheldrick,1997) _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0600P)^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 3042 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1367 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1296 _refine_ls_wR_factor_gt 0.1090 _refine_ls_goodness_of_fit_ref 0.840 _refine_ls_restrained_S_all 0.840 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.0000 0.10846(7) 0.2500 0.0769(3) Uani 1 2 d S . . Cl1 Cl 0.07113(7) 0.13293(19) 0.16257(10) 0.1094(6) Uani 1 1 d . . . N1 N -0.04624(19) -0.0292(5) 0.1912(2) 0.0721(12) Uani 1 1 d . . . H1A H -0.0419 -0.1261 0.1992 0.086 Uiso 1 1 d R . . C31 C -0.1818(3) -0.1189(6) 0.1351(4) 0.0717(15) Uani 1 1 d . . . O3 O -0.0991(2) -0.2138(4) 0.0784(2) 0.0904(12) Uani 1 1 d . . . C2 C -0.0848(2) 0.0183(6) 0.1399(3) 0.0673(15) Uani 1 1 d . . . O2 O -0.14491(18) -0.0133(5) 0.0254(2) 0.0934(12) Uani 1 1 d . . . C4 C -0.1508(3) 0.1361(7) 0.0210(4) 0.0854(17) Uani 1 1 d . . . C3 C -0.1269(3) -0.0820(6) 0.0961(3) 0.0793(17) Uani 1 1 d . . . C32 C -0.2244(3) -0.2104(7) 0.1005(4) 0.096(2) Uani 1 1 d . . . H32A H -0.2180 -0.2514 0.0527 0.116 Uiso 1 1 d R . . C36 C -0.1931(3) -0.0640(7) 0.2021(5) 0.100(2) Uani 1 1 d . . . H36A H -0.1647 0.0005 0.2270 0.120 Uiso 1 1 d R . . C35 C -0.2454(3) -0.0954(8) 0.2358(4) 0.115(2) Uani 1 1 d . . . H35A H -0.2526 -0.0549 0.2835 0.139 Uiso 1 1 d R . . C5 C -0.1821(3) 0.1881(9) -0.0432(4) 0.108(2) Uani 1 1 d . . . H5A H -0.1992 0.1221 -0.0801 0.130 Uiso 1 1 d R . . C6 C -0.1887(3) 0.3344(10) -0.0521(5) 0.122(3) Uani 1 1 d . . . H6A H -0.2093 0.3704 -0.0965 0.147 Uiso 1 1 d R . . C34 C -0.2869(3) -0.1871(9) 0.2010(6) 0.115(2) Uani 1 1 d . . . H34A H -0.3231 -0.2104 0.2240 0.137 Uiso 1 1 d R . . C33 C -0.2758(4) -0.2439(7) 0.1330(6) 0.113(3) Uani 1 1 d . . . H33A H -0.3048 -0.3079 0.1087 0.136 Uiso 1 1 d R . . C10 C -0.0466(4) -0.1960(8) 0.0343(4) 0.127(3) Uani 1 1 d . . . H10A H -0.0168 -0.1396 0.0621 0.152 Uiso 1 1 d R . . H10B H -0.0570 -0.1447 -0.0111 0.152 Uiso 1 1 d R . . O1 O -0.05594(18) 0.2492(4) 0.1781(2) 0.0886(12) Uani 1 1 d . . . C1 C -0.0881(3) 0.1744(7) 0.1336(4) 0.0748(16) Uani 1 1 d . . . C8 C -0.1342(3) 0.3836(7) 0.0622(4) 0.101(2) Uani 1 1 d . . . H8A H -0.1187 0.4512 0.0993 0.121 Uiso 1 1 d R . . C9 C -0.1258(3) 0.2324(7) 0.0732(4) 0.0813(17) Uani 1 1 d . . . C7 C -0.1650(3) 0.4333(8) -0.0006(5) 0.122(3) Uani 1 1 d . . . H7A H -0.1712 0.5363 -0.0083 0.146 Uiso 1 1 d R . . C11 C -0.0278(6) -0.3333(13) 0.0115(8) 0.152(5) Uiso 0.70 1 d P . . H11A H 0.0063 -0.3204 -0.0173 0.228 Uiso 0.70 1 d PR . . H11B H -0.0173 -0.3952 0.0533 0.228 Uiso 0.70 1 d PR . . H11C H -0.0594 -0.3780 -0.0187 0.228 Uiso 0.70 1 d PR . . C11' C 0.0030(16) -0.295(3) 0.0557(19) 0.165(12) Uiso 0.30 1 d P . . H11E H 0.0335 -0.2724 0.0225 0.248 Uiso 0.30 1 d PR . . H11F H 0.0194 -0.2891 0.1060 0.248 Uiso 0.30 1 d PR . . H11D H -0.0118 -0.3919 0.0459 0.248 Uiso 0.30 1 d PR . . O1W O 0.0000 0.6907(7) 0.2500 0.154(3) Uani 1 2 d S . . O2W O 0.0760(7) 0.5203(19) 0.1987(9) 0.259(7) Uani 0.50 1 d P . . 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 0.0598(5) 0.0783(5) 0.0904(6) 0.000 -0.0126(4) 0.000 Cl1 0.0778(12) 0.1444(14) 0.1054(14) 0.0161(11) 0.0005(10) -0.0183(10) N1 0.067(3) 0.070(3) 0.079(3) -0.001(2) -0.001(3) 0.000(2) C31 0.066(4) 0.076(4) 0.071(4) 0.001(3) -0.005(4) 0.000(3) O3 0.081(3) 0.098(3) 0.092(3) -0.014(2) 0.004(3) -0.001(2) C2 0.053(4) 0.083(4) 0.065(4) 0.006(3) -0.007(3) -0.011(3) O2 0.108(3) 0.091(3) 0.078(3) 0.006(2) -0.023(3) -0.014(2) C4 0.075(4) 0.089(5) 0.090(5) 0.016(4) -0.008(4) -0.006(4) C3 0.082(5) 0.081(5) 0.073(4) -0.003(4) -0.010(4) 0.000(4) C32 0.070(5) 0.110(5) 0.107(5) -0.023(4) -0.012(4) -0.005(4) C36 0.078(5) 0.110(5) 0.112(6) -0.010(4) 0.000(5) -0.014(4) C35 0.086(5) 0.153(6) 0.108(6) -0.014(5) 0.010(5) -0.029(5) C5 0.108(6) 0.113(6) 0.099(6) 0.017(4) -0.035(5) -0.005(4) C6 0.114(6) 0.128(6) 0.120(7) 0.031(5) -0.031(5) 0.013(5) C34 0.079(5) 0.118(5) 0.145(8) 0.017(5) -0.004(6) -0.018(5) C33 0.079(6) 0.105(5) 0.153(8) -0.010(5) -0.014(6) -0.020(4) C10 0.153(8) 0.124(6) 0.104(6) -0.019(5) 0.016(6) 0.022(6) O1 0.080(3) 0.075(3) 0.106(3) 0.004(2) -0.029(3) -0.002(2) C1 0.056(4) 0.077(4) 0.090(5) 0.006(4) -0.003(4) -0.005(3) C8 0.087(5) 0.089(5) 0.122(6) 0.011(4) -0.020(4) 0.003(4) C9 0.069(4) 0.081(5) 0.091(5) 0.006(4) -0.017(4) -0.007(3) C7 0.112(6) 0.108(6) 0.140(7) 0.028(5) -0.039(6) 0.008(4) O1W 0.194(8) 0.111(5) 0.152(6) 0.000 -0.036(6) 0.000 O2W 0.223(16) 0.296(16) 0.263(17) 0.085(15) 0.054(14) 0.091(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 1.910(4) . ? Ru1 N1 1.910(4) 2 ? Ru1 O1 2.171(4) 2 ? Ru1 O1 2.171(4) . ? Ru1 Cl1 2.3261(18) . ? Ru1 Cl1 2.3261(18) 2 ? N1 C2 1.302(6) . ? C31 C36 1.348(8) . ? C31 C32 1.389(8) . ? C31 C3 1.496(8) . ? O3 C3 1.402(6) . ? O3 C10 1.475(8) . ? C2 C1 1.431(7) . ? C2 C3 1.506(7) . ? O2 C4 1.371(6) . ? O2 C3 1.457(6) . ? C4 C9 1.382(7) . ? C4 C5 1.402(8) . ? C32 C33 1.364(9) . ? C36 C35 1.386(8) . ? C35 C34 1.376(9) . ? C5 C6 1.351(9) . ? C6 C7 1.379(9) . ? C34 C33 1.369(9) . ? C10 C11 1.393(12) . ? C10 C11' 1.47(3) . ? O1 C1 1.250(6) . ? C1 C9 1.441(8) . ? C8 C7 1.368(8) . ? C8 C9 1.405(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N1 97.7(3) . 2 ? N1 Ru1 O1 175.14(18) . 2 ? N1 Ru1 O1 77.41(18) 2 2 ? N1 Ru1 O1 77.41(18) . . ? N1 Ru1 O1 175.14(18) 2 . ? O1 Ru1 O1 107.4(2) 2 . ? N1 Ru1 Cl1 93.41(13) . . ? N1 Ru1 Cl1 93.83(13) 2 . ? O1 Ru1 Cl1 87.22(12) 2 . ? O1 Ru1 Cl1 86.27(12) . . ? N1 Ru1 Cl1 93.83(13) . 2 ? N1 Ru1 Cl1 93.41(13) 2 2 ? O1 Ru1 Cl1 86.27(12) 2 2 ? O1 Ru1 Cl1 87.22(12) . 2 ? Cl1 Ru1 Cl1 168.98(9) . 2 ? C2 N1 Ru1 119.4(4) . . ? C36 C31 C32 117.6(6) . . ? C36 C31 C3 123.0(6) . . ? C32 C31 C3 119.3(6) . . ? C3 O3 C10 114.3(5) . . ? N1 C2 C1 114.7(5) . . ? N1 C2 C3 122.7(5) . . ? C1 C2 C3 122.4(6) . . ? C4 O2 C3 119.9(5) . . ? O2 C4 C9 124.0(6) . . ? O2 C4 C5 115.2(6) . . ? C9 C4 C5 120.7(6) . . ? O3 C3 O2 105.8(5) . . ? O3 C3 C31 107.9(5) . . ? O2 C3 C31 108.5(5) . . ? O3 C3 C2 111.5(5) . . ? O2 C3 C2 109.3(4) . . ? C31 C3 C2 113.6(5) . . ? C33 C32 C31 121.3(7) . . ? C31 C36 C35 121.9(6) . . ? C34 C35 C36 119.7(7) . . ? C6 C5 C4 118.6(7) . . ? C5 C6 C7 122.1(7) . . ? C33 C34 C35 118.9(8) . . ? C32 C33 C34 120.5(7) . . ? C11 C10 C11' 44.4(13) . . ? C11 C10 O3 109.1(8) . . ? C11' C10 O3 114.3(14) . . ? C1 O1 Ru1 110.6(4) . . ? O1 C1 C2 117.9(6) . . ? O1 C1 C9 125.2(6) . . ? C2 C1 C9 116.8(6) . . ? C7 C8 C9 119.9(7) . . ? C4 C9 C8 118.9(6) . . ? C4 C9 C1 118.6(6) . . ? C8 C9 C1 122.4(6) . . ? C8 C7 C6 119.7(7) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.545 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.065 # Attachment '- comp_1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 779230' #TrackingRef '- comp_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis-dichloridobis(3-imino-2-methoxyflavanone)ruthenium(II) x 3H2O ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H26 Cl2 N2 O6 Ru, 3 H2 O' _chemical_formula_sum 'C32 H32 Cl2 N2 O9 Ru' _chemical_formula_weight 760.57 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall '-C 2yc' 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 22.434(4) _cell_length_b 8.694(8) _cell_length_c 17.63(1) _cell_angle_alpha 90.00 _cell_angle_beta 93.56(3) _cell_angle_gamma 90.00 _cell_volume 3432(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.90 _cell_measurement_theta_max 14.75 _chemical_compound_source 'chemical synthesis' _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.666 _exptl_absorpt_correction_type Analytical _exptl_absorpt_process_details '(De Meulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.750 _exptl_absorpt_correction_T_max 0.842 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'AFC5S Rigaku' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.27 _diffrn_reflns_number 7803 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.0791 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3938 _reflns_number_gt 2828 _reflns_threshold_expression >2\s(I) loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -4 0 2 1 1 2 -5 1 1 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale 1 1.000 2 2.130 3 5.040 4 10.140 _computing_data_collection 'MSC/AFC Diffractometer Control Software (1989)' _computing_cell_refinement 'MSC/AFC Diffractometer Control Software (1989)' _computing_data_reduction 'CRYSTAL STRUCTURE (2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2005)' _computing_publication_material 'PLATON (Spek, 2005)' _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^)+(0.0537P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3938 _refine_ls_number_parameters 213 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1114 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.0000 0.58809(4) 0.2500 0.03812(13) Uani 1 2 d S . . Cl1 Cl -0.07534(4) 0.61281(13) 0.15328(5) 0.0652(3) Uani 1 1 d . . . O1 O 0.05261(9) 0.7358(3) 0.18033(12) 0.0480(5) Uani 1 1 d . . . O2 O 0.12794(10) 0.4594(3) 0.02598(12) 0.0491(5) Uani 1 1 d . . . O3 O 0.09286(11) 0.2456(3) 0.08359(13) 0.0567(6) Uani 1 1 d . . . N1 N 0.04357(10) 0.4431(3) 0.19331(13) 0.0410(6) Uani 1 1 d . . . H1A H 0.0399 0.3462 0.2015 0.049 Uiso 1 1 calc R . . C1 C 0.08121(12) 0.6552(4) 0.13551(16) 0.0396(6) Uani 1 1 d . . . C2 C 0.07848(12) 0.4913(3) 0.14274(16) 0.0388(7) Uani 1 1 d . . . C3 C 0.11837(14) 0.3888(4) 0.09918(18) 0.0448(7) Uani 1 1 d . . . C4 C 0.13703(14) 0.6146(4) 0.02269(18) 0.0479(8) Uani 1 1 d . . . C5 C 0.16678(17) 0.6693(5) -0.0385(2) 0.0619(9) Uani 1 1 d . . . H5A H 0.1804 0.6013 -0.0744 0.074 Uiso 1 1 calc R . . C6 C 0.1759(2) 0.8234(5) -0.0457(2) 0.0781(12) Uani 1 1 d . . . H6A H 0.1960 0.8595 -0.0867 0.094 Uiso 1 1 calc R . . C7 C 0.1561(2) 0.9274(5) 0.0063(2) 0.0810(13) Uani 1 1 d . . . H7A H 0.1630 1.0321 0.0003 0.097 Uiso 1 1 calc R . . C8 C 0.12605(18) 0.8754(4) 0.0671(2) 0.0609(10) Uani 1 1 d . . . H8A H 0.1125 0.9449 0.1022 0.073 Uiso 1 1 calc R . . C9 C 0.11600(13) 0.7174(4) 0.07588(17) 0.0455(7) Uani 1 1 d . . . C10 C 0.03573(17) 0.2476(5) 0.0382(2) 0.0715(11) Uani 1 1 d . . . H10A H 0.0076 0.3102 0.0632 0.107 Uiso 1 1 calc R . . H10B H 0.0205 0.1446 0.0330 0.107 Uiso 1 1 calc R . . H10C H 0.0416 0.2892 -0.0112 0.107 Uiso 1 1 calc R . . C31 C 0.17870(15) 0.3629(4) 0.14097(19) 0.0504(8) Uani 1 1 d . . . C32 C 0.22492(16) 0.3048(5) 0.1014(2) 0.0669(10) Uani 1 1 d . . . H32A H 0.2184 0.2833 0.0499 0.080 Uiso 1 1 calc R . . C33 C 0.28046(16) 0.2781(6) 0.1365(3) 0.0798(13) Uani 1 1 d . . . H33A H 0.3107 0.2365 0.1090 0.096 Uiso 1 1 calc R . . C34 C 0.29106(19) 0.3126(8) 0.2112(3) 0.1041(19) Uani 1 1 d . . . H34A H 0.3285 0.2936 0.2351 0.125 Uiso 1 1 calc R . . C35 C 0.2471(2) 0.3749(9) 0.2512(3) 0.132(3) Uani 1 1 d . . . H35A H 0.2547 0.4003 0.3021 0.158 Uiso 1 1 calc R . . C36 C 0.1906(2) 0.4005(7) 0.2160(2) 0.100(2) Uani 1 1 d . . . H36A H 0.1607 0.4435 0.2436 0.120 Uiso 1 1 calc R . . O1W O 0.0000 0.1568(6) 0.2500 0.1044(16) Uani 1 2 d SD . . H1W H 0.027(2) 0.084(5) 0.277(3) 0.13(2) Uiso 1 1 d D . . O2W O 0.0579(3) 0.9793(8) 0.3516(5) 0.239(3) 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 0.02386(16) 0.0449(2) 0.0459(2) 0.000 0.00422(12) 0.000 Cl1 0.0406(4) 0.0944(7) 0.0593(5) 0.0049(5) -0.0081(4) 0.0075(4) O1 0.0414(11) 0.0472(13) 0.0569(13) -0.0020(10) 0.0146(9) 0.0019(10) O2 0.0551(13) 0.0481(13) 0.0451(12) 0.0002(10) 0.0108(10) 0.0005(11) O3 0.0589(14) 0.0449(13) 0.0672(14) -0.0055(11) 0.0101(11) -0.0003(11) N1 0.0353(12) 0.0401(15) 0.0480(14) 0.0029(10) 0.0056(10) 0.0003(10) C1 0.0271(13) 0.0482(17) 0.0434(16) -0.0002(13) 0.0009(11) 0.0010(12) C2 0.0304(14) 0.0422(18) 0.0435(16) 0.0006(12) 0.0012(12) 0.0028(12) C3 0.0433(16) 0.0419(18) 0.0501(17) -0.0021(13) 0.0109(13) 0.0037(14) C4 0.0382(15) 0.055(2) 0.0508(17) 0.0037(14) 0.0034(13) -0.0009(14) C5 0.065(2) 0.067(3) 0.056(2) 0.0023(18) 0.0213(17) -0.003(2) C6 0.088(3) 0.070(3) 0.080(3) 0.015(2) 0.036(2) -0.012(2) C7 0.099(3) 0.057(3) 0.091(3) 0.008(2) 0.036(3) -0.015(2) C8 0.066(2) 0.046(2) 0.072(2) -0.0014(16) 0.0193(19) -0.0041(17) C9 0.0348(14) 0.0488(19) 0.0532(18) 0.0021(15) 0.0049(13) -0.0014(14) C10 0.068(2) 0.067(3) 0.079(3) -0.015(2) 0.002(2) -0.020(2) C31 0.0421(16) 0.0533(19) 0.0565(19) 0.0040(15) 0.0084(14) 0.0109(15) C32 0.0474(19) 0.083(3) 0.071(2) -0.004(2) 0.0135(17) 0.013(2) C33 0.0432(19) 0.099(3) 0.099(3) 0.000(3) 0.014(2) 0.022(2) C34 0.053(2) 0.160(6) 0.098(4) 0.005(4) -0.001(2) 0.050(3) C35 0.080(3) 0.230(8) 0.082(3) -0.020(4) -0.019(3) 0.069(5) C36 0.060(2) 0.171(6) 0.070(3) -0.017(3) 0.000(2) 0.052(3) O1W 0.133(5) 0.067(3) 0.115(4) 0.000 0.028(4) 0.000 O2W 0.240(8) 0.139(5) 0.326(8) -0.033(6) -0.074(7) 0.018(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 Ru1 N1 1.914(3) . ? Ru1 N1 1.914(3) 2 ? Ru1 O1 2.175(2) . ? Ru1 O1 2.175(2) 2 ? Ru1 Cl1 2.3351(12) 2 ? Ru1 Cl1 2.3351(12) . ? O1 C1 1.261(4) . ? O2 C4 1.366(4) . ? O2 C3 1.457(4) . ? O3 C3 1.391(4) . ? O3 C10 1.468(4) . ? N1 C2 1.292(4) . ? N1 H1A 0.8600 . ? C1 C2 1.432(5) . ? C1 C9 1.452(4) . ? C2 C3 1.507(4) . ? C3 C31 1.517(5) . ? C4 C5 1.388(5) . ? C4 C9 1.398(4) . ? C5 C6 1.362(6) . ? C5 H5A 0.9300 . ? C6 C7 1.380(6) . ? C6 H6A 0.9300 . ? C7 C8 1.378(5) . ? C7 H7A 0.9300 . ? C8 C9 1.402(5) . ? C8 H8A 0.9300 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C31 C36 1.373(5) . ? C31 C32 1.381(5) . ? C32 C33 1.376(5) . ? C32 H32A 0.9300 . ? C33 C34 1.358(6) . ? C33 H33A 0.9300 . ? C34 C35 1.361(7) . ? C34 H34A 0.9300 . ? C35 C36 1.395(6) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? O1W H1W 0.98(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N1 97.65(15) . 2 ? N1 Ru1 O1 77.37(11) . . ? N1 Ru1 O1 175.00(9) 2 . ? N1 Ru1 O1 175.00(9) . 2 ? N1 Ru1 O1 77.37(11) 2 2 ? O1 Ru1 O1 107.62(12) . 2 ? N1 Ru1 Cl1 94.13(8) . 2 ? N1 Ru1 Cl1 92.82(8) 2 2 ? O1 Ru1 Cl1 87.96(7) . 2 ? O1 Ru1 Cl1 85.81(7) 2 2 ? N1 Ru1 Cl1 92.82(8) . . ? N1 Ru1 Cl1 94.12(8) 2 . ? O1 Ru1 Cl1 85.81(7) . . ? O1 Ru1 Cl1 87.96(7) 2 . ? Cl1 Ru1 Cl1 169.44(6) 2 . ? C1 O1 Ru1 109.9(2) . . ? C4 O2 C3 119.0(2) . . ? C3 O3 C10 115.6(3) . . ? C2 N1 Ru1 119.8(2) . . ? C2 N1 H1A 120.1 . . ? Ru1 N1 H1A 120.1 . . ? O1 C1 C2 118.1(3) . . ? O1 C1 C9 124.3(3) . . ? C2 C1 C9 117.6(3) . . ? N1 C2 C1 114.5(3) . . ? N1 C2 C3 124.4(3) . . ? C1 C2 C3 120.9(3) . . ? O3 C3 O2 106.5(2) . . ? O3 C3 C2 112.3(3) . . ? O2 C3 C2 109.1(2) . . ? O3 C3 C31 107.9(3) . . ? O2 C3 C31 108.5(3) . . ? C2 C3 C31 112.4(3) . . ? O2 C4 C5 116.9(3) . . ? O2 C4 C9 123.0(3) . . ? C5 C4 C9 120.1(3) . . ? C6 C5 C4 119.4(4) . . ? C6 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C5 C6 C7 121.8(4) . . ? C5 C6 H6A 119.1 . . ? C7 C6 H6A 119.1 . . ? C8 C7 C6 119.6(4) . . ? C8 C7 H7A 120.2 . . ? C6 C7 H7A 120.2 . . ? C7 C8 C9 119.8(4) . . ? C7 C8 H8A 120.1 . . ? C9 C8 H8A 120.1 . . ? C4 C9 C8 119.3(3) . . ? C4 C9 C1 117.8(3) . . ? C8 C9 C1 122.8(3) . . ? O3 C10 H10A 109.5 . . ? O3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C36 C31 C32 117.9(3) . . ? C36 C31 C3 123.1(3) . . ? C32 C31 C3 119.0(3) . . ? C33 C32 C31 121.5(4) . . ? C33 C32 H32A 119.3 . . ? C31 C32 H32A 119.3 . . ? C34 C33 C32 119.9(4) . . ? C34 C33 H33A 120.1 . . ? C32 C33 H33A 120.1 . . ? C33 C34 C35 120.1(4) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? C34 C35 C36 120.1(5) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C31 C36 C35 120.5(4) . . ? C31 C36 H36A 119.8 . . ? C35 C36 H36A 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ru1 O1 C1 4.34(18) . . . . ? O1 Ru1 O1 C1 -176.0(2) 2 . . . ? Cl1 Ru1 O1 C1 99.03(18) 2 . . . ? Cl1 Ru1 O1 C1 -89.50(18) . . . . ? N1 Ru1 N1 C2 176.9(3) 2 . . . ? O1 Ru1 N1 C2 -2.8(2) . . . . ? Cl1 Ru1 N1 C2 -89.7(2) 2 . . . ? Cl1 Ru1 N1 C2 82.3(2) . . . . ? Ru1 O1 C1 C2 -5.3(3) . . . . ? Ru1 O1 C1 C9 173.5(2) . . . . ? Ru1 N1 C2 C1 0.9(3) . . . . ? Ru1 N1 C2 C3 175.1(2) . . . . ? O1 C1 C2 N1 3.4(4) . . . . ? C9 C1 C2 N1 -175.5(2) . . . . ? O1 C1 C2 C3 -171.0(3) . . . . ? C9 C1 C2 C3 10.1(4) . . . . ? C10 O3 C3 O2 -59.6(3) . . . . ? C10 O3 C3 C2 59.8(4) . . . . ? C10 O3 C3 C31 -175.8(3) . . . . ? C4 O2 C3 O3 162.3(3) . . . . ? C4 O2 C3 C2 40.8(4) . . . . ? C4 O2 C3 C31 -81.9(3) . . . . ? N1 C2 C3 O3 34.7(4) . . . . ? C1 C2 C3 O3 -151.5(3) . . . . ? N1 C2 C3 O2 152.5(3) . . . . ? C1 C2 C3 O2 -33.6(4) . . . . ? N1 C2 C3 C31 -87.2(4) . . . . ? C1 C2 C3 C31 86.7(3) . . . . ? C3 O2 C4 C5 157.1(3) . . . . ? C3 O2 C4 C9 -25.3(4) . . . . ? O2 C4 C5 C6 178.5(4) . . . . ? C9 C4 C5 C6 0.8(6) . . . . ? C4 C5 C6 C7 -0.3(7) . . . . ? C5 C6 C7 C8 -0.2(8) . . . . ? C6 C7 C8 C9 0.2(7) . . . . ? O2 C4 C9 C8 -178.4(3) . . . . ? C5 C4 C9 C8 -0.9(5) . . . . ? O2 C4 C9 C1 -2.2(5) . . . . ? C5 C4 C9 C1 175.4(3) . . . . ? C7 C8 C9 C4 0.4(6) . . . . ? C7 C8 C9 C1 -175.7(4) . . . . ? O1 C1 C9 C4 -169.5(3) . . . . ? C2 C1 C9 C4 9.3(4) . . . . ? O1 C1 C9 C8 6.6(5) . . . . ? C2 C1 C9 C8 -174.6(3) . . . . ? O3 C3 C31 C36 -111.3(4) . . . . ? O2 C3 C31 C36 133.8(4) . . . . ? C2 C3 C31 C36 13.1(5) . . . . ? O3 C3 C31 C32 71.6(4) . . . . ? O2 C3 C31 C32 -43.3(4) . . . . ? C2 C3 C31 C32 -164.0(3) . . . . ? C36 C31 C32 C33 3.1(7) . . . . ? C3 C31 C32 C33 -179.6(4) . . . . ? C31 C32 C33 C34 -1.6(8) . . . . ? C32 C33 C34 C35 -0.6(10) . . . . ? C33 C34 C35 C36 1.3(11) . . . . ? C32 C31 C36 C35 -2.4(8) . . . . ? C3 C31 C36 C35 -179.6(5) . . . . ? C34 C35 C36 C31 0.2(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1A O1W 1_555 0.86 2.08 2.876(6) 153 yes O1W H1W O2W 1_545 0.98(5) 1.71(5) 2.644(9) 158(4) yes _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.694 _refine_diff_density_min -1.394 _refine_diff_density_rms 0.091