# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email agajw@yahoo.com _publ_contact_author_name 'Agnieszka Jablonska - Wawrzycka' loop_ _publ_author_name 'Agnieszka Jablonska-Wawrzycka' 'Patrycja Rogala' 'Maciej Hodorowicz' 'Slawomir Michalkiewicz' ; B.Barszcz ; data_(1) _database_code_depnum_ccdc_archive 'CCDC 902426' #TrackingRef '(1).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(2,2'-pirydyliumbenzimidazolium)dichloride bis[(bisacetonitrile) tetrachlororuthenate(III)] (bisacetonitrile)tetrachlororythenium(IV) hexahydrate ; _chemical_name_common ; bis(2,2'-pirydyliumbenzimidazolium)dichloride bis((bisacetonitrile) tetrachlororuthenate(iii)) (bisacetonitrile)tetrachlororythenium(IV) hexahydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C36 H40 Cl14 N12 O6 Ru3' _chemical_formula_sum 'C36 H40 Cl14 N12 O6 Ru3' _chemical_formula_weight 1536.31 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.157(5) _cell_length_b 9.634(5) _cell_length_c 19.943(5) _cell_angle_alpha 78.397(5) _cell_angle_beta 78.995(5) _cell_angle_gamma 82.639(5) _cell_volume 1500.4(13) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10646 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description column _exptl_crystal_colour orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 758 _exptl_absorpt_coefficient_mu 1.418 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6518 _exptl_absorpt_correction_T_max 0.8049 _exptl_absorpt_process_details 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _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 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \o scans to fill Ewald sphere' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19818 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.45 _reflns_number_total 6686 _reflns_number_gt 5271 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+0.0417P] 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 SHELXL _refine_ls_extinction_coef 0.0055(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6686 _refine_ls_number_parameters 338 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.050 _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 0.89990(3) 0.19805(2) 0.304820(10) 0.03242(9) Uani 1 1 d . . . Ru2 Ru 0.5000 0.0000 0.0000 0.03601(10) Uani 1 2 d S . . Cl0 Cl 0.34326(9) 0.69330(8) 0.31287(4) 0.04904(19) Uani 1 1 d . . . C9 C 0.7022(3) 0.6744(2) 0.43474(13) 0.0307(5) Uani 1 1 d . . . C10 C 0.8952(3) 0.7082(2) 0.25346(13) 0.0305(5) Uani 1 1 d . . . N11 N 1.0568(3) 0.7177(2) 0.22456(11) 0.0344(5) Uani 1 1 d . . . C12 C 1.1081(4) 0.7356(3) 0.15653(14) 0.0440(7) Uani 1 1 d . . . H12 H 1.2211 0.7432 0.1383 0.053 Uiso 1 1 calc R . . C13 C 0.9953(4) 0.7431(3) 0.11310(15) 0.0490(7) Uani 1 1 d . . . H13 H 1.0308 0.7555 0.0653 0.059 Uiso 1 1 calc R . . C14 C 0.8295(4) 0.7321(3) 0.14054(15) 0.0506(8) Uani 1 1 d . . . H14 H 0.7517 0.7364 0.1115 0.061 Uiso 1 1 calc R . . C15 C 0.7781(3) 0.7147(3) 0.21149(14) 0.0412(6) Uani 1 1 d . . . H15 H 0.6656 0.7074 0.2307 0.049 Uiso 1 1 calc R . . C4 C 0.5774(3) 0.6623(3) 0.49368(14) 0.0389(6) Uani 1 1 d . . . H4 H 0.4649 0.6627 0.4908 0.047 Uiso 1 1 calc R . . C5 C 0.6307(4) 0.6499(3) 0.55602(14) 0.0459(7) Uani 1 1 d . . . H5 H 0.5519 0.6406 0.5966 0.055 Uiso 1 1 calc R . . C6 C 0.7999(4) 0.6506(3) 0.56061(15) 0.0468(7) Uani 1 1 d . . . H6 H 0.8299 0.6417 0.6041 0.056 Uiso 1 1 calc R . . C7 C 0.9224(4) 0.6641(3) 0.50276(14) 0.0428(7) Uani 1 1 d . . . H7 H 1.0347 0.6653 0.5056 0.051 Uiso 1 1 calc R . . C8 C 0.8688(3) 0.6759(3) 0.43960(13) 0.0342(6) Uani 1 1 d . . . C2 C 0.8509(3) 0.6940(2) 0.32901(13) 0.0290(5) Uani 1 1 d . . . Cl2 Cl 1.00174(12) 0.05909(9) 0.21814(5) 0.0653(2) Uani 1 1 d . . . N2 N 1.0633(3) 0.0885(2) 0.36544(12) 0.0400(5) Uani 1 1 d . . . Cl3 Cl 0.70331(10) 0.03723(8) 0.35975(4) 0.0548(2) Uani 1 1 d . . . Cl4 Cl 0.80147(9) 0.34209(7) 0.38783(3) 0.04153(17) Uani 1 1 d . . . Cl1 Cl 1.09999(10) 0.36079(8) 0.25104(4) 0.05150(19) Uani 1 1 d . . . N4 N 0.7339(3) 0.3095(2) 0.24593(12) 0.0414(5) Uani 1 1 d . . . N5 N 0.4794(3) 0.0164(3) 0.10090(12) 0.0430(6) Uani 1 1 d . . . N1 N 0.9577(3) 0.6882(2) 0.37263(11) 0.0334(5) Uani 1 1 d . . . Cl5 Cl 0.51394(10) 0.24792(8) -0.03236(4) 0.05111(19) Uani 1 1 d . . . N3 N 0.6957(3) 0.6869(2) 0.36516(11) 0.0307(5) Uani 1 1 d D . . Cl6 Cl 0.20693(9) 0.03188(9) 0.01258(4) 0.0521(2) Uani 1 1 d . . . C21 C 1.1530(4) 0.0328(3) 0.40129(15) 0.0443(7) Uani 1 1 d . . . C41 C 0.6409(4) 0.3710(3) 0.21354(15) 0.0447(7) Uani 1 1 d . . . C22 C 1.2695(4) -0.0367(4) 0.44723(19) 0.0671(10) Uani 1 1 d . . . H22A H 1.3792 -0.0062 0.4286 0.101 Uiso 1 1 calc R . . H22B H 1.2737 -0.1380 0.4511 0.101 Uiso 1 1 calc R . . H22C H 1.2325 -0.0119 0.4923 0.101 Uiso 1 1 calc R . . C42 C 0.5194(4) 0.4484(4) 0.17173(19) 0.0681(10) Uani 1 1 d . . . H42A H 0.5454 0.5453 0.1564 0.102 Uiso 1 1 calc R . . H42B H 0.4090 0.4463 0.1991 0.102 Uiso 1 1 calc R . . H42C H 0.5235 0.4048 0.1321 0.102 Uiso 1 1 calc R . . C51 C 0.4652(4) 0.0306(3) 0.15672(15) 0.0411(6) Uani 1 1 d . . . C52 C 0.4483(5) 0.0506(3) 0.22804(14) 0.0567(8) Uani 1 1 d . . . H52A H 0.5568 0.0589 0.2381 0.085 Uiso 1 1 calc R . . H52B H 0.4005 -0.0296 0.2589 0.085 Uiso 1 1 calc R . . H52C H 0.3764 0.1358 0.2343 0.085 Uiso 1 1 calc R . . O1 O 0.8112(4) 0.2102(4) 0.08435(18) 0.1122(12) Uani 1 1 d U . . O2 O 0.7821(6) 0.6534(5) -0.0887(2) 0.1563(17) Uani 1 1 d U . . O3 O 0.8618(8) 0.4771(7) 0.0231(3) 0.224(3) Uani 1 1 d U . . H1 H 1.066(4) 0.693(3) 0.3614(14) 0.039(8) Uiso 1 1 d . . . H3 H 0.605(3) 0.685(3) 0.3472(15) 0.055(9) Uiso 1 1 d D . . H11 H 1.138(5) 0.711(4) 0.2470(19) 0.076(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 Ru1 0.03697(15) 0.02505(12) 0.03696(14) -0.00446(8) -0.01286(9) -0.00123(9) Ru2 0.03243(19) 0.0465(2) 0.02637(16) 0.00291(12) -0.00693(12) -0.00591(13) Cl0 0.0260(4) 0.0653(5) 0.0547(4) 0.0013(3) -0.0133(3) -0.0099(3) C9 0.0317(14) 0.0243(12) 0.0369(14) -0.0044(10) -0.0089(11) -0.0032(10) C10 0.0268(14) 0.0259(12) 0.0380(14) -0.0010(10) -0.0090(11) -0.0015(10) N11 0.0268(13) 0.0377(12) 0.0397(13) -0.0051(9) -0.0084(10) -0.0053(9) C12 0.0320(16) 0.0523(18) 0.0420(16) 0.0004(13) 0.0006(12) -0.0071(13) C13 0.054(2) 0.0600(19) 0.0315(15) 0.0002(13) -0.0086(13) -0.0103(15) C14 0.049(2) 0.067(2) 0.0374(16) 0.0017(14) -0.0191(14) -0.0128(15) C15 0.0315(15) 0.0532(17) 0.0395(15) -0.0024(12) -0.0103(12) -0.0095(12) C4 0.0327(15) 0.0377(15) 0.0436(16) -0.0030(12) -0.0053(12) -0.0018(11) C5 0.0482(19) 0.0475(17) 0.0391(16) -0.0061(12) -0.0019(13) -0.0049(13) C6 0.0511(19) 0.0505(17) 0.0430(16) -0.0104(13) -0.0152(14) -0.0067(14) C7 0.0381(17) 0.0516(17) 0.0429(16) -0.0109(13) -0.0126(13) -0.0072(13) C8 0.0324(15) 0.0349(14) 0.0369(14) -0.0082(11) -0.0078(11) -0.0039(11) C2 0.0245(14) 0.0270(12) 0.0371(13) -0.0052(10) -0.0107(11) -0.0008(10) Cl2 0.0841(6) 0.0526(5) 0.0670(5) -0.0330(4) -0.0185(5) 0.0079(4) N2 0.0420(14) 0.0324(12) 0.0465(13) -0.0062(10) -0.0133(11) -0.0002(10) Cl3 0.0571(5) 0.0406(4) 0.0688(5) 0.0064(3) -0.0230(4) -0.0200(3) Cl4 0.0384(4) 0.0440(4) 0.0452(4) -0.0162(3) -0.0095(3) 0.0012(3) Cl1 0.0492(5) 0.0428(4) 0.0580(5) -0.0035(3) 0.0010(3) -0.0119(3) N4 0.0486(15) 0.0344(12) 0.0439(13) -0.0038(10) -0.0174(12) -0.0048(11) N5 0.0402(14) 0.0536(15) 0.0327(13) 0.0011(10) -0.0079(10) -0.0067(11) N1 0.0202(12) 0.0445(13) 0.0369(12) -0.0067(9) -0.0075(9) -0.0059(9) Cl5 0.0530(5) 0.0472(4) 0.0482(4) 0.0049(3) -0.0085(3) -0.0078(3) N3 0.0248(12) 0.0314(11) 0.0376(12) -0.0047(9) -0.0105(9) -0.0037(9) Cl6 0.0324(4) 0.0680(5) 0.0499(4) 0.0050(3) -0.0087(3) -0.0049(3) C21 0.0433(18) 0.0383(15) 0.0491(17) -0.0030(13) -0.0102(14) -0.0003(13) C41 0.0448(18) 0.0434(16) 0.0440(16) 0.0031(13) -0.0109(14) -0.0096(13) C22 0.059(2) 0.063(2) 0.073(2) 0.0134(18) -0.0321(19) 0.0062(17) C42 0.053(2) 0.070(2) 0.072(2) 0.0220(18) -0.0271(18) -0.0036(17) C51 0.0403(17) 0.0448(16) 0.0367(16) -0.0008(12) -0.0064(12) -0.0087(12) C52 0.081(3) 0.0539(19) 0.0394(17) -0.0100(14) -0.0137(16) -0.0140(17) O1 0.093(2) 0.154(3) 0.108(2) -0.062(2) -0.0102(19) -0.027(2) O2 0.168(4) 0.193(5) 0.110(3) -0.062(3) -0.003(3) 0.001(3) O3 0.252(7) 0.202(5) 0.225(6) -0.119(5) 0.042(5) -0.041(5) _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 N4 2.023(2) . ? Ru1 N2 2.023(2) . ? Ru1 Cl4 2.3328(9) . ? Ru1 Cl3 2.3356(11) . ? Ru1 Cl2 2.3597(10) . ? Ru1 Cl1 2.3628(11) . ? Ru2 N5 2.023(2) . ? Ru2 N5 2.023(2) 2_655 ? Ru2 Cl6 2.3422(16) . ? Ru2 Cl6 2.3422(16) 2_655 ? Ru2 Cl5 2.3571(14) 2_655 ? Ru2 Cl5 2.3571(14) . ? C9 N3 1.379(3) . ? C9 C8 1.382(4) . ? C9 C4 1.396(4) . ? C10 N11 1.341(3) . ? C10 C15 1.374(3) . ? C10 C2 1.463(3) . ? N11 C12 1.324(3) . ? N11 H11 0.86(4) . ? C12 C13 1.366(4) . ? C12 H12 0.9300 . ? C13 C14 1.368(4) . ? C13 H13 0.9300 . ? C14 C15 1.379(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C4 C5 1.372(4) . ? C4 H4 0.9300 . ? C5 C6 1.401(4) . ? C5 H5 0.9300 . ? C6 C7 1.371(4) . ? C6 H6 0.9300 . ? C7 C8 1.390(4) . ? C7 H7 0.9300 . ? C8 N1 1.383(3) . ? C2 N1 1.333(3) . ? C2 N3 1.334(3) . ? N2 C21 1.131(3) . ? N4 C41 1.123(4) . ? N5 C51 1.131(3) . ? N1 H1 0.87(3) . ? N3 H3 0.889(17) . ? C21 C22 1.454(4) . ? C41 C42 1.452(4) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C51 C52 1.452(4) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ru1 N2 178.78(9) . . ? N4 Ru1 Cl4 89.22(7) . . ? N2 Ru1 Cl4 89.60(7) . . ? N4 Ru1 Cl3 90.64(8) . . ? N2 Ru1 Cl3 89.09(8) . . ? Cl4 Ru1 Cl3 90.62(4) . . ? N4 Ru1 Cl2 89.79(7) . . ? N2 Ru1 Cl2 91.40(7) . . ? Cl4 Ru1 Cl2 178.12(3) . . ? Cl3 Ru1 Cl2 90.99(4) . . ? N4 Ru1 Cl1 90.04(8) . . ? N2 Ru1 Cl1 90.21(8) . . ? Cl4 Ru1 Cl1 88.74(4) . . ? Cl3 Ru1 Cl1 179.06(3) . . ? Cl2 Ru1 Cl1 89.66(4) . . ? N5 Ru2 N5 180.0 . 2_655 ? N5 Ru2 Cl6 88.71(7) . . ? N5 Ru2 Cl6 91.29(7) 2_655 . ? N5 Ru2 Cl6 91.29(7) . 2_655 ? N5 Ru2 Cl6 88.71(7) 2_655 2_655 ? Cl6 Ru2 Cl6 180.0 . 2_655 ? N5 Ru2 Cl5 90.24(7) . 2_655 ? N5 Ru2 Cl5 89.76(7) 2_655 2_655 ? Cl6 Ru2 Cl5 89.52(3) . 2_655 ? Cl6 Ru2 Cl5 90.48(3) 2_655 2_655 ? N5 Ru2 Cl5 89.76(7) . . ? N5 Ru2 Cl5 90.24(7) 2_655 . ? Cl6 Ru2 Cl5 90.48(3) . . ? Cl6 Ru2 Cl5 89.52(3) 2_655 . ? Cl5 Ru2 Cl5 180.0 2_655 . ? N3 C9 C8 106.7(2) . . ? N3 C9 C4 132.0(2) . . ? C8 C9 C4 121.4(2) . . ? N11 C10 C15 119.3(2) . . ? N11 C10 C2 118.0(2) . . ? C15 C10 C2 122.7(2) . . ? C12 N11 C10 122.4(2) . . ? C12 N11 H11 112(2) . . ? C10 N11 H11 125(2) . . ? N11 C12 C13 120.0(3) . . ? N11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C14 119.4(3) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C13 C14 C15 119.7(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C10 C15 C14 119.1(3) . . ? C10 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C5 C4 C9 116.0(3) . . ? C5 C4 H4 122.0 . . ? C9 C4 H4 122.0 . . ? C4 C5 C6 122.3(3) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C7 C6 C5 121.8(3) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 C7 C8 116.0(3) . . ? C6 C7 H7 122.0 . . ? C8 C7 H7 122.0 . . ? C9 C8 N1 106.6(2) . . ? C9 C8 C7 122.5(2) . . ? N1 C8 C7 130.9(3) . . ? N1 C2 N3 109.1(2) . . ? N1 C2 C10 125.8(2) . . ? N3 C2 C10 125.1(2) . . ? C21 N2 Ru1 176.4(2) . . ? C41 N4 Ru1 179.5(3) . . ? C51 N5 Ru2 177.4(2) . . ? C2 N1 C8 108.8(2) . . ? C2 N1 H1 126.4(18) . . ? C8 N1 H1 124.8(18) . . ? C2 N3 C9 108.9(2) . . ? C2 N3 H3 125(2) . . ? C9 N3 H3 126(2) . . ? N2 C21 C22 179.1(3) . . ? N4 C41 C42 179.1(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N5 C51 C52 179.2(3) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 C10 N11 C12 1.2(4) . . . . ? C2 C10 N11 C12 -177.6(2) . . . . ? C10 N11 C12 C13 -1.0(4) . . . . ? N11 C12 C13 C14 0.1(5) . . . . ? C12 C13 C14 C15 0.5(5) . . . . ? N11 C10 C15 C14 -0.6(4) . . . . ? C2 C10 C15 C14 178.2(3) . . . . ? C13 C14 C15 C10 -0.2(5) . . . . ? N3 C9 C4 C5 179.2(3) . . . . ? C8 C9 C4 C5 -1.0(4) . . . . ? C9 C4 C5 C6 0.6(4) . . . . ? C4 C5 C6 C7 0.1(5) . . . . ? C5 C6 C7 C8 -0.5(4) . . . . ? N3 C9 C8 N1 -0.4(3) . . . . ? C4 C9 C8 N1 179.7(2) . . . . ? N3 C9 C8 C7 -179.5(2) . . . . ? C4 C9 C8 C7 0.7(4) . . . . ? C6 C7 C8 C9 0.1(4) . . . . ? C6 C7 C8 N1 -178.7(3) . . . . ? N11 C10 C2 N1 -0.6(4) . . . . ? C15 C10 C2 N1 -179.5(2) . . . . ? N11 C10 C2 N3 178.3(2) . . . . ? C15 C10 C2 N3 -0.5(4) . . . . ? N4 Ru1 N2 C21 -28(7) . . . . ? Cl4 Ru1 N2 C21 -15(4) . . . . ? Cl3 Ru1 N2 C21 -105(4) . . . . ? Cl2 Ru1 N2 C21 164(4) . . . . ? Cl1 Ru1 N2 C21 74(4) . . . . ? N2 Ru1 N4 C41 -63(32) . . . . ? Cl4 Ru1 N4 C41 -76(31) . . . . ? Cl3 Ru1 N4 C41 15(31) . . . . ? Cl2 Ru1 N4 C41 105(31) . . . . ? Cl1 Ru1 N4 C41 -165(100) . . . . ? N5 Ru2 N5 C51 -86(11) 2_655 . . . ? Cl6 Ru2 N5 C51 -63(5) . . . . ? Cl6 Ru2 N5 C51 117(5) 2_655 . . . ? Cl5 Ru2 N5 C51 -153(5) 2_655 . . . ? Cl5 Ru2 N5 C51 27(5) . . . . ? N3 C2 N1 C8 0.4(3) . . . . ? C10 C2 N1 C8 179.5(2) . . . . ? C9 C8 N1 C2 0.0(3) . . . . ? C7 C8 N1 C2 179.0(3) . . . . ? N1 C2 N3 C9 -0.7(3) . . . . ? C10 C2 N3 C9 -179.8(2) . . . . ? C8 C9 N3 C2 0.7(3) . . . . ? C4 C9 N3 C2 -179.5(3) . . . . ? Ru1 N2 C21 C22 -48(26) . . . . ? Ru1 N4 C41 C42 -44(50) . . . . ? Ru2 N5 C51 C52 -57(31) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1 Cl0 0.87(3) 2.29(3) 3.146(3) 169(2) 1_655 y N3 H3 Cl0 0.889(17) 2.347(18) 3.230(3) 172(3) . y N11 H11 Cl0 0.86(4) 2.28(4) 3.143(3) 177(3) 1_655 y _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.599 _refine_diff_density_min -0.770 _refine_diff_density_rms 0.098 # Attachment '(2).cif' data_(2) _database_code_depnum_ccdc_archive 'CCDC 902427' #TrackingRef '(2).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; mer-(acetonitrile)(trichloro)(2,2'-pyrydylbenzimidazole)ruthenium(III) 2,2'-pirydylbenzimidazole solvate trihydrate ; _chemical_name_common ; mer-(acetonitrile)(trichloro)(2,2'- pyrydylbenzimidazole)ruthenium(iii) 2,2'-pirydylbenzimidazole solvate trihydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H21 Cl3 N7 O3 Ru' _chemical_formula_weight 686.92 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' Cl Cl 0.1484 0.1585 '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 35.6130(11) _cell_length_b 14.3500(4) _cell_length_c 13.7450(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.207(2) _cell_angle_gamma 90.00 _cell_volume 6548.6(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 110426 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 24.407 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 0.760 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8753 _exptl_absorpt_correction_T_max 0.8945 _exptl_absorpt_process_details 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _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 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \o scans to fill Ewald sphere' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42524 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 24.39 _reflns_number_total 5360 _reflns_number_gt 4691 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1050P)^2^+69.7851P] 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 SHELXL _refine_ls_extinction_coef 0.0011(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5360 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.2101 _refine_ls_wR_factor_gt 0.1994 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 0.305698(16) 0.08604(3) 0.81822(4) 0.0395(3) Uani 1 1 d . . . Cl1 Cl 0.25778(5) -0.00881(10) 0.69616(12) 0.0423(4) Uani 1 1 d . . . Cl3 Cl 0.35277(6) 0.18498(13) 0.93652(15) 0.0557(5) Uani 1 1 d . . . Cl2 Cl 0.31966(6) -0.03422(12) 0.94431(14) 0.0550(5) Uani 1 1 d . . . C2 C 0.25788(19) 0.2423(4) 0.7199(5) 0.0345(13) Uani 1 1 d . . . N1 N 0.29013(17) 0.1944(3) 0.7173(4) 0.0382(12) Uani 1 1 d . . . N11 N 0.25981(18) 0.1447(4) 0.8567(4) 0.0422(13) Uani 1 1 d . . . N3 N 0.24883(18) 0.3141(4) 0.6517(4) 0.0413(13) Uani 1 1 d . . . C8 C 0.3027(2) 0.2371(4) 0.6447(5) 0.0400(14) Uani 1 1 d . . . C9 C 0.2767(2) 0.3138(4) 0.6018(5) 0.0376(14) Uani 1 1 d . . . N40 N 0.3513 0.0280 0.7732 0.0521(17) Uani 1 1 d . . . C10 C 0.2397(2) 0.2170(4) 0.7951(5) 0.0435(15) Uani 1 1 d . . . C12 C 0.2467(2) 0.1178(5) 0.9336(5) 0.0498(18) Uani 1 1 d . . . H12 H 0.2601 0.0695 0.9776 0.060 Uiso 1 1 calc R . . C7 C 0.3346(2) 0.2184(5) 0.6129(5) 0.0465(16) Uani 1 1 d . . . H7 H 0.3520 0.1687 0.6396 0.056 Uiso 1 1 calc R . . C15 C 0.2072(2) 0.2602(5) 0.8041(6) 0.0474(16) Uani 1 1 d . . . H15 H 0.1940 0.3081 0.7591 0.057 Uiso 1 1 calc R . . C4 C 0.2812(2) 0.3716(5) 0.5271(5) 0.0498(17) Uani 1 1 d . . . H4 H 0.2638 0.4210 0.4993 0.060 Uiso 1 1 calc R . . C5 C 0.3127(3) 0.3527(5) 0.4958(6) 0.057(2) Uani 1 1 d . . . H5 H 0.3167 0.3899 0.4450 0.069 Uiso 1 1 calc R . . C14 C 0.1942(3) 0.2297(6) 0.8844(6) 0.058(2) Uani 1 1 d . . . H14 H 0.1721 0.2574 0.8935 0.069 Uiso 1 1 calc R . . C6 C 0.3390(2) 0.2789(5) 0.5382(6) 0.0528(18) Uani 1 1 d . . . H6 H 0.3604 0.2695 0.5157 0.063 Uiso 1 1 calc R . . C13 C 0.2147(3) 0.1586(5) 0.9491(6) 0.057(2) Uani 1 1 d . . . H13 H 0.2068 0.1385 1.0031 0.068 Uiso 1 1 calc R . . C22 C 0.4768(3) 0.5175(7) 0.8669(5) 0.063(2) Uani 1 1 d . . . C29 C 0.4191(2) 0.4505(9) 0.8417(5) 0.070(3) Uani 1 1 d . . . C41 C 0.3675 -0.0011 0.7346 0.098(4) Uani 1 1 d . . . N21 N 0.4522(3) 0.5868(7) 0.8554(6) 0.082(2) Uani 1 1 d . . . H21 H 0.4580 0.6451 0.8577 0.098 Uiso 1 1 calc R . . N23 N 0.4610(3) 0.4357(7) 0.8618(6) 0.085(3) Uani 1 1 d . . . C28 C 0.4133(3) 0.5472(8) 0.8380(6) 0.069(3) Uani 1 1 d . . . C25 C 0.3503(3) 0.4316(8) 0.8060(6) 0.070(3) Uani 1 1 d . . . H25 H 0.3278 0.3943 0.7956 0.084 Uiso 1 1 calc R . . C24 C 0.3866(3) 0.3906(7) 0.8251(6) 0.072(3) Uani 1 1 d . . . H24 H 0.3896 0.3261 0.8270 0.086 Uiso 1 1 calc R . . C26 C 0.3461(3) 0.5238(8) 0.8016(6) 0.068(3) Uani 1 1 d . . . H26 H 0.3202 0.5467 0.7871 0.082 Uiso 1 1 calc R . . C42 C 0.3970 -0.0447 0.6844 0.144(7) Uani 1 1 d . . . H42A H 0.3842 -0.0453 0.6098 0.216 Uiso 1 1 calc R . . H42B H 0.4038 -0.1072 0.7093 0.216 Uiso 1 1 calc R . . H42C H 0.4212 -0.0079 0.7036 0.216 Uiso 1 1 calc R . . O1 O 0.4391(2) 0.1850(6) 0.6265(13) 0.176(6) Uani 1 1 d . . . O3 O 0.4505(5) 0.2203(7) 0.3392(13) 0.192(6) Uani 1 1 d . . . O2 O 0.5154(5) 0.2604(9) 0.6268(16) 0.211(8) Uani 1 1 d . . . C33 C 0.5987(4) 0.542(2) 0.9137(8) 0.127(8) Uani 1 1 d . . . H33 H 0.6259 0.5417 0.9235 0.153 Uiso 1 1 calc R . . C30 C 0.5219(3) 0.5282(12) 0.8853(6) 0.085(4) Uani 1 1 d . . . C32 C 0.5775(7) 0.6340(15) 0.9080(8) 0.142(8) Uani 1 1 d . . . H32 H 0.5900 0.6918 0.9143 0.170 Uiso 1 1 calc R . . N31 N 0.5331(4) 0.6206(11) 0.8907(7) 0.120(4) Uani 1 1 d . . . C35 C 0.5427(4) 0.4574(11) 0.8908(7) 0.090(3) Uani 1 1 d . . . H35 H 0.5313 0.3984 0.8844 0.108 Uiso 1 1 calc R . . C34 C 0.5799(5) 0.4672(16) 0.9053(8) 0.120(6) Uani 1 1 d . . . H34 H 0.5947 0.4128 0.9102 0.144 Uiso 1 1 calc R . . C27 C 0.3757 0.5880 0.8163 0.072(3) Uani 1 1 d . . . H27 H 0.3713 0.6520 0.8123 0.086 Uiso 1 1 calc R . . H3 H 0.224(3) 0.362(7) 0.642(7) 0.08(3) 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 0.0496(4) 0.0253(3) 0.0407(4) 0.0031(2) 0.0129(3) -0.0014(2) Cl1 0.0610(10) 0.0236(7) 0.0391(8) -0.0003(6) 0.0143(7) -0.0021(6) Cl3 0.0594(11) 0.0496(10) 0.0526(10) -0.0008(8) 0.0137(8) -0.0175(8) Cl2 0.0641(11) 0.0406(9) 0.0490(10) 0.0133(8) 0.0069(8) -0.0098(8) C2 0.050(3) 0.024(3) 0.031(3) -0.003(2) 0.016(3) -0.004(3) N1 0.056(3) 0.025(3) 0.035(3) 0.000(2) 0.019(2) -0.003(2) N11 0.064(4) 0.029(3) 0.036(3) -0.005(2) 0.021(3) -0.012(2) N3 0.059(3) 0.027(3) 0.039(3) 0.002(2) 0.019(3) 0.002(2) C8 0.056(4) 0.029(3) 0.036(3) -0.009(3) 0.018(3) -0.009(3) C9 0.056(4) 0.026(3) 0.029(3) -0.004(2) 0.014(3) -0.006(3) N40 0.082(5) 0.034(3) 0.057(4) 0.003(3) 0.045(4) -0.002(3) C10 0.055(4) 0.032(3) 0.042(4) -0.005(3) 0.015(3) -0.008(3) C12 0.079(5) 0.039(4) 0.037(4) -0.006(3) 0.028(4) -0.020(4) C7 0.059(4) 0.041(4) 0.042(4) -0.009(3) 0.022(3) -0.007(3) C15 0.061(4) 0.033(3) 0.051(4) -0.008(3) 0.023(3) -0.004(3) C4 0.076(5) 0.036(4) 0.036(3) -0.003(3) 0.019(3) -0.013(3) C5 0.096(6) 0.041(4) 0.037(4) -0.003(3) 0.026(4) -0.019(4) C14 0.071(5) 0.049(4) 0.065(5) -0.017(4) 0.038(4) -0.014(4) C6 0.071(5) 0.049(4) 0.047(4) -0.009(3) 0.030(4) -0.012(4) C13 0.080(5) 0.050(4) 0.051(4) -0.014(4) 0.038(4) -0.022(4) C22 0.085(6) 0.078(6) 0.027(4) 0.003(4) 0.019(4) -0.016(5) C29 0.042(4) 0.146(10) 0.024(3) 0.006(5) 0.013(3) 0.018(5) C41 0.092(8) 0.053(6) 0.101(8) 0.023(6) -0.022(7) -0.010(5) N21 0.102(6) 0.090(6) 0.049(4) 0.005(4) 0.023(4) 0.000(5) N23 0.098(6) 0.107(7) 0.048(4) 0.006(4) 0.025(4) 0.017(5) C28 0.069(5) 0.105(8) 0.031(4) -0.005(4) 0.017(4) -0.040(6) C25 0.064(5) 0.107(8) 0.038(4) -0.017(5) 0.016(4) -0.030(5) C24 0.103(8) 0.073(6) 0.042(4) -0.007(4) 0.029(5) -0.003(5) C26 0.053(5) 0.110(8) 0.038(4) -0.009(5) 0.014(4) 0.007(5) C42 0.096(9) 0.215(18) 0.127(12) 0.001(12) 0.049(9) 0.063(11) O1 0.056(4) 0.082(6) 0.383(19) 0.017(8) 0.070(8) -0.007(4) O3 0.272(17) 0.077(7) 0.227(15) 0.004(8) 0.087(13) 0.005(9) O2 0.221(14) 0.114(8) 0.36(2) -0.081(11) 0.180(15) -0.079(9) C33 0.056(6) 0.30(3) 0.028(5) 0.004(10) 0.015(4) -0.037(11) C30 0.063(6) 0.165(13) 0.023(4) -0.001(6) 0.012(4) -0.024(7) C32 0.210(19) 0.175(16) 0.034(5) -0.020(8) 0.036(8) -0.123(15) N31 0.134(10) 0.172(12) 0.045(5) 0.006(6) 0.022(6) 0.022(9) C35 0.086(8) 0.132(10) 0.045(5) 0.005(6) 0.016(5) 0.020(8) C34 0.093(10) 0.23(2) 0.039(6) 0.019(8) 0.022(6) 0.046(11) C27 0.090(7) 0.082(7) 0.044(5) 0.000(4) 0.025(5) -0.002(5) _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 2.023(5) . ? Ru1 N11 2.070(6) . ? Ru1 N40 2.1080(6) . ? Ru1 Cl3 2.3447(18) . ? Ru1 Cl1 2.3469(16) . ? Ru1 Cl2 2.3677(17) . ? C2 N3 1.350(8) . ? C2 N1 1.350(8) . ? C2 C10 1.450(9) . ? N1 C8 1.377(8) . ? N11 C12 1.357(9) . ? N11 C10 1.366(9) . ? N3 C9 1.397(9) . ? N3 H3 1.10(10) . ? C8 C7 1.383(10) . ? C8 C9 1.421(9) . ? C9 C4 1.373(9) . ? N40 C41 1.0039 . ? C10 C15 1.358(10) . ? C12 C13 1.365(11) . ? C12 H12 0.9300 . ? C7 C6 1.396(10) . ? C7 H7 0.9300 . ? C15 C14 1.412(11) . ? C15 H15 0.9300 . ? C4 C5 1.365(12) . ? C4 H4 0.9300 . ? C5 C6 1.394(12) . ? C5 H5 0.9300 . ? C14 C13 1.376(12) . ? C14 H14 0.9300 . ? C6 H6 0.9300 . ? C13 H13 0.9300 . ? C22 N23 1.292(13) . ? C22 N21 1.297(13) . ? C22 C30 1.541(13) . ? C29 C24 1.392(15) . ? C29 C28 1.401(15) . ? C29 N23 1.434(12) . ? C41 C42 1.5814 . ? N21 C28 1.435(12) . ? N21 H21 0.8600 . ? C28 C27 1.391(11) . ? C25 C26 1.331(14) . ? C25 C24 1.357(14) . ? C25 H25 0.9300 . ? C24 H24 0.9300 . ? C26 C27 1.360(11) . ? C26 H26 0.9300 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C33 C34 1.25(2) . ? C33 C32 1.50(3) . ? C33 H33 0.9300 . ? C30 C35 1.243(18) . ? C30 N31 1.380(19) . ? C32 N31 1.52(2) . ? C32 H32 0.9300 . ? C35 C34 1.274(19) . ? C35 H35 0.9300 . ? C34 H34 0.9300 . ? C27 H27 0.9300 . ? 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 N11 79.5(2) . . ? N1 Ru1 N40 98.69(15) . . ? N11 Ru1 N40 177.84(15) . . ? N1 Ru1 Cl3 87.71(16) . . ? N11 Ru1 Cl3 90.50(15) . . ? N40 Ru1 Cl3 90.53(6) . . ? N1 Ru1 Cl1 90.43(15) . . ? N11 Ru1 Cl1 88.95(15) . . ? N40 Ru1 Cl1 89.96(5) . . ? Cl3 Ru1 Cl1 178.13(6) . . ? N1 Ru1 Cl2 174.29(16) . . ? N11 Ru1 Cl2 94.90(16) . . ? N40 Ru1 Cl2 86.97(6) . . ? Cl3 Ru1 Cl2 91.46(7) . . ? Cl1 Ru1 Cl2 90.37(6) . . ? N3 C2 N1 111.2(5) . . ? N3 C2 C10 129.1(6) . . ? N1 C2 C10 119.6(5) . . ? C2 N1 C8 107.1(5) . . ? C2 N1 Ru1 113.5(4) . . ? C8 N1 Ru1 139.4(5) . . ? C12 N11 C10 116.7(6) . . ? C12 N11 Ru1 127.5(5) . . ? C10 N11 Ru1 115.8(4) . . ? C2 N3 C9 107.8(5) . . ? C2 N3 H3 123(5) . . ? C9 N3 H3 129(5) . . ? N1 C8 C7 131.4(6) . . ? N1 C8 C9 108.2(6) . . ? C7 C8 C9 120.3(6) . . ? C4 C9 N3 131.4(7) . . ? C4 C9 C8 122.9(7) . . ? N3 C9 C8 105.7(5) . . ? C41 N40 Ru1 165.796(14) . . ? C15 C10 N11 124.2(6) . . ? C15 C10 C2 124.4(6) . . ? N11 C10 C2 111.4(6) . . ? N11 C12 C13 122.8(7) . . ? N11 C12 H12 118.6 . . ? C13 C12 H12 118.6 . . ? C8 C7 C6 115.8(7) . . ? C8 C7 H7 122.1 . . ? C6 C7 H7 122.1 . . ? C10 C15 C14 117.4(7) . . ? C10 C15 H15 121.3 . . ? C14 C15 H15 121.3 . . ? C5 C4 C9 116.5(7) . . ? C5 C4 H4 121.7 . . ? C9 C4 H4 121.7 . . ? C4 C5 C6 121.6(7) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C13 C14 C15 119.2(7) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C5 C6 C7 122.8(7) . . ? C5 C6 H6 118.6 . . ? C7 C6 H6 118.6 . . ? C12 C13 C14 119.6(7) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? N23 C22 N21 115.4(10) . . ? N23 C22 C30 120.4(11) . . ? N21 C22 C30 124.2(11) . . ? C24 C29 C28 120.2(8) . . ? C24 C29 N23 133.3(11) . . ? C28 C29 N23 106.5(10) . . ? N40 C41 C42 173.854(1) . . ? C22 N21 C28 106.6(9) . . ? C22 N21 H21 126.7 . . ? C28 N21 H21 126.7 . . ? C22 N23 C29 106.1(10) . . ? C27 C28 C29 122.9(7) . . ? C27 C28 N21 131.7(10) . . ? C29 C28 N21 105.4(9) . . ? C26 C25 C24 121.7(9) . . ? C26 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? C25 C24 C29 116.1(10) . . ? C25 C24 H24 121.9 . . ? C29 C24 H24 121.9 . . ? C25 C26 C27 126.7(8) . . ? C25 C26 H26 116.7 . . ? C27 C26 H26 116.7 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C34 C33 C32 120.6(13) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C35 C30 N31 128.9(12) . . ? C35 C30 C22 119.5(14) . . ? N31 C30 C22 111.6(13) . . ? C33 C32 N31 111.8(12) . . ? C33 C32 H32 124.1 . . ? N31 C32 H32 124.1 . . ? C30 N31 C32 113.1(13) . . ? C30 C35 C34 118.9(17) . . ? C30 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C33 C34 C35 126.7(18) . . ? C33 C34 H34 116.6 . . ? C35 C34 H34 116.6 . . ? C26 C27 C28 112.4(6) . . ? C26 C27 H27 123.8 . . ? C28 C27 H27 123.8 . . ? 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 N3 C2 N1 C8 0.3(7) . . . . ? C10 C2 N1 C8 -175.8(5) . . . . ? N3 C2 N1 Ru1 179.7(4) . . . . ? C10 C2 N1 Ru1 3.6(7) . . . . ? N11 Ru1 N1 C2 -4.8(4) . . . . ? N40 Ru1 N1 C2 174.1(4) . . . . ? Cl3 Ru1 N1 C2 -95.7(4) . . . . ? Cl1 Ru1 N1 C2 84.1(4) . . . . ? Cl2 Ru1 N1 C2 -13.9(19) . . . . ? N11 Ru1 N1 C8 174.3(7) . . . . ? N40 Ru1 N1 C8 -6.8(6) . . . . ? Cl3 Ru1 N1 C8 83.4(6) . . . . ? Cl1 Ru1 N1 C8 -96.8(6) . . . . ? Cl2 Ru1 N1 C8 165.1(12) . . . . ? N1 Ru1 N11 C12 -176.7(6) . . . . ? N40 Ru1 N11 C12 152(4) . . . . ? Cl3 Ru1 N11 C12 -89.1(5) . . . . ? Cl1 Ru1 N11 C12 92.6(5) . . . . ? Cl2 Ru1 N11 C12 2.4(5) . . . . ? N1 Ru1 N11 C10 5.6(4) . . . . ? N40 Ru1 N11 C10 -25(4) . . . . ? Cl3 Ru1 N11 C10 93.2(4) . . . . ? Cl1 Ru1 N11 C10 -85.1(4) . . . . ? Cl2 Ru1 N11 C10 -175.3(4) . . . . ? N1 C2 N3 C9 -0.3(7) . . . . ? C10 C2 N3 C9 175.3(6) . . . . ? C2 N1 C8 C7 178.3(7) . . . . ? Ru1 N1 C8 C7 -0.8(11) . . . . ? C2 N1 C8 C9 -0.2(7) . . . . ? Ru1 N1 C8 C9 -179.3(5) . . . . ? C2 N3 C9 C4 -179.4(7) . . . . ? C2 N3 C9 C8 0.2(7) . . . . ? N1 C8 C9 C4 179.6(6) . . . . ? C7 C8 C9 C4 1.0(10) . . . . ? N1 C8 C9 N3 0.0(7) . . . . ? C7 C8 C9 N3 -178.7(6) . . . . ? N1 Ru1 N40 C41 -59.93(16) . . . . ? N11 Ru1 N40 C41 -29(4) . . . . ? Cl3 Ru1 N40 C41 -147.70(6) . . . . ? Cl1 Ru1 N40 C41 30.50(7) . . . . ? Cl2 Ru1 N40 C41 120.87(6) . . . . ? C12 N11 C10 C15 -2.3(9) . . . . ? Ru1 N11 C10 C15 175.7(5) . . . . ? C12 N11 C10 C2 176.9(5) . . . . ? Ru1 N11 C10 C2 -5.1(7) . . . . ? N3 C2 C10 C15 4.9(11) . . . . ? N1 C2 C10 C15 -179.8(6) . . . . ? N3 C2 C10 N11 -174.3(6) . . . . ? N1 C2 C10 N11 1.0(8) . . . . ? C10 N11 C12 C13 1.1(10) . . . . ? Ru1 N11 C12 C13 -176.6(5) . . . . ? N1 C8 C7 C6 -178.2(6) . . . . ? C9 C8 C7 C6 0.1(9) . . . . ? N11 C10 C15 C14 1.8(10) . . . . ? C2 C10 C15 C14 -177.3(6) . . . . ? N3 C9 C4 C5 178.8(6) . . . . ? C8 C9 C4 C5 -0.8(10) . . . . ? C9 C4 C5 C6 -0.5(10) . . . . ? C10 C15 C14 C13 0.0(10) . . . . ? C4 C5 C6 C7 1.6(11) . . . . ? C8 C7 C6 C5 -1.3(10) . . . . ? N11 C12 C13 C14 0.5(11) . . . . ? C15 C14 C13 C12 -1.1(11) . . . . ? Ru1 N40 C41 C42 171.08(5) . . . . ? N23 C22 N21 C28 -1.0(10) . . . . ? C30 C22 N21 C28 178.8(7) . . . . ? N21 C22 N23 C29 1.3(10) . . . . ? C30 C22 N23 C29 -178.5(6) . . . . ? C24 C29 N23 C22 177.7(8) . . . . ? C28 C29 N23 C22 -1.0(9) . . . . ? C24 C29 C28 C27 -1.1(11) . . . . ? N23 C29 C28 C27 177.8(6) . . . . ? C24 C29 C28 N21 -178.5(7) . . . . ? N23 C29 C28 N21 0.4(8) . . . . ? C22 N21 C28 C27 -176.7(7) . . . . ? C22 N21 C28 C29 0.3(9) . . . . ? C26 C25 C24 C29 1.1(12) . . . . ? C28 C29 C24 C25 -0.1(11) . . . . ? N23 C29 C24 C25 -178.6(8) . . . . ? C24 C25 C26 C27 -1.0(13) . . . . ? N23 C22 C30 C35 3.0(12) . . . . ? N21 C22 C30 C35 -176.8(9) . . . . ? N23 C22 C30 N31 -178.6(8) . . . . ? N21 C22 C30 N31 1.6(11) . . . . ? C34 C33 C32 N31 -0.6(15) . . . . ? C35 C30 N31 C32 -1.4(14) . . . . ? C22 C30 N31 C32 -179.6(7) . . . . ? C33 C32 N31 C30 0.8(12) . . . . ? N31 C30 C35 C34 1.4(16) . . . . ? C22 C30 C35 C34 179.6(8) . . . . ? C32 C33 C34 C35 0.7(19) . . . . ? C30 C35 C34 C33 -1.0(18) . . . . ? C25 C26 C27 C28 -0.2(10) . . . . ? C29 C28 C27 C26 1.3(9) . . . . ? N21 C28 C27 C26 177.8(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N21 H21 O3 0.86 1.95 2.777(14) 159.6 6_566 y N3 H3 Cl2 1.10(10) 2.16(10) 3.179(6) 153(7) 4_556 y N3 H3 Cl1 1.10(10) 2.78(9) 3.354(6) 112(6) 4_556 y _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.39 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.909 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.142 # Attachment '(3).cif' data_(3) _database_code_depnum_ccdc_archive 'CCDC 902428' #TrackingRef '(3).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis(2-hydroxymethylbenzimidazolium) dichloride hexachlororuthenate(IV) tetrahydrate ; _chemical_name_common ; tetrakis(2-hydroxymethylbenzimidazolium) dichloride hexachlororuthenate(IV) tetrahydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H40 Cl8 N8 O8 Ru' _chemical_formula_weight 1049.39 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.024(5) _cell_length_b 9.673(5) _cell_length_c 16.021(5) _cell_angle_alpha 84.899(5) _cell_angle_beta 88.419(5) _cell_angle_gamma 86.979(5) _cell_volume 1082.4(10) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12704 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description column _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8386 _exptl_absorpt_correction_T_max 0.9306 _exptl_absorpt_process_details 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _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 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \o scans to fill Ewald sphere' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16640 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4935 _reflns_number_gt 4611 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+2.9243P] 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 SHELXL _refine_ls_extinction_coef 0.038(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4935 _refine_ls_number_parameters 264 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1886 _refine_ls_wR_factor_gt 0.1857 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.011 _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 O31 O 0.4874(14) 0.2688(7) 0.1217(6) 0.137(3) Uani 1 1 d U . . H31 H 0.3825 0.2916 0.1022 0.205 Uiso 1 1 calc R . . N21 N 0.5831(7) 0.0878(5) 0.2677(4) 0.0631(14) Uani 1 1 d . . . H21 H 0.5886 0.1726 0.2793 0.076 Uiso 1 1 calc R . . N23 N 0.5563(6) -0.0921(5) 0.1977(4) 0.0564(12) Uani 1 1 d . . . H23 H 0.5425 -0.1418 0.1566 0.068 Uiso 1 1 calc R . . C22 C 0.5499(8) 0.0474(6) 0.1926(5) 0.0618(16) Uani 1 1 d . . . C30 C 0.534(2) 0.1382(11) 0.1071(9) 0.137(3) Uani 1 1 d U . . H30A H 0.6556 0.1338 0.0766 0.164 Uiso 1 1 calc R . . H30B H 0.4384 0.1032 0.0733 0.164 Uiso 1 1 calc R . . C29 C 0.5890(7) -0.1429(5) 0.2803(4) 0.0503(12) Uani 1 1 d . . . C26 C 0.6522(11) -0.1743(7) 0.4487(5) 0.0687(17) Uani 1 1 d . . . H26 H 0.6737 -0.1878 0.5060 0.082 Uiso 1 1 calc R . . C24 C 0.6022(9) -0.2780(6) 0.3183(5) 0.0603(15) Uani 1 1 d . . . H24 H 0.5913 -0.3554 0.2885 0.072 Uiso 1 1 calc R . . C27 C 0.6402(10) -0.0409(7) 0.4100(5) 0.0642(16) Uani 1 1 d . . . H27 H 0.6532 0.0366 0.4394 0.077 Uiso 1 1 calc R . . C28 C 0.6077(8) -0.0293(6) 0.3249(4) 0.0542(13) Uani 1 1 d . . . C25 C 0.6326(10) -0.2887(7) 0.4035(5) 0.0672(17) Uani 1 1 d . . . H25 H 0.6405 -0.3768 0.4321 0.081 Uiso 1 1 calc R . . O11 O 0.1397(7) 0.4358(4) 0.3795(2) 0.0581(10) Uani 1 1 d . . . H11 H 0.2540 0.4137 0.3789 0.087 Uiso 1 1 calc R . . N1 N 0.0584(6) 0.7167(4) 0.2139(3) 0.0435(9) Uani 1 1 d . . . H1 H 0.0404 0.6862 0.1661 0.052 Uiso 1 1 calc R . . N3 N 0.1122(6) 0.7195(4) 0.3462(2) 0.0405(8) Uani 1 1 d . . . H3 H 0.1339 0.6914 0.3977 0.049 Uiso 1 1 calc R . . C10 C 0.0837(10) 0.4839(6) 0.2983(4) 0.0565(14) Uani 1 1 d . . . H10A H -0.0436 0.4547 0.2893 0.068 Uiso 1 1 calc R . . H10B H 0.1697 0.4432 0.2577 0.068 Uiso 1 1 calc R . . C9 C 0.0994(6) 0.8566(5) 0.3132(3) 0.0385(9) Uani 1 1 d . . . C6 C 0.0574(9) 1.1000(6) 0.2131(4) 0.0554(13) Uani 1 1 d . . . H6 H 0.0449 1.1841 0.1802 0.066 Uiso 1 1 calc R . . C2 C 0.0853(7) 0.6380(5) 0.2851(3) 0.0411(10) Uani 1 1 d . . . C8 C 0.0638(6) 0.8552(5) 0.2283(3) 0.0382(9) Uani 1 1 d . . . C4 C 0.1133(8) 0.9800(6) 0.3506(4) 0.0515(12) Uani 1 1 d . . . H4 H 0.1371 0.9806 0.4074 0.062 Uiso 1 1 calc R . . C5 C 0.0901(9) 1.1016(6) 0.2989(4) 0.0599(14) Uani 1 1 d . . . H5 H 0.0962 1.1864 0.3216 0.072 Uiso 1 1 calc R . . C7 C 0.0433(7) 0.9785(5) 0.1759(3) 0.0471(11) Uani 1 1 d . . . H7 H 0.0214 0.9781 0.1190 0.056 Uiso 1 1 calc R . . Ru1 Ru 0.0000 0.5000 0.0000 0.0329(2) Uani 1 2 d S . . Cl1 Cl -0.19183(19) 0.46649(14) 0.12244(8) 0.0504(3) Uani 1 1 d . . . Cl3 Cl -0.2651(3) 0.5214(2) -0.08027(12) 0.0793(5) Uani 1 1 d . . . Cl2 Cl -0.0257(2) 0.74390(12) 0.01122(8) 0.0514(3) Uani 1 1 d . . . O0A O 0.1352(8) -0.3046(7) 0.5143(3) 0.0800(15) Uani 1 1 d D . . Cl0 Cl 0.4436(3) -0.36160(16) 0.65254(11) 0.0646(4) Uani 1 1 d . . . O0B O -0.4931(8) 0.2758(6) -0.0798(3) 0.0852(16) Uani 1 1 d . . . H0AB H 0.195(14) -0.377(9) 0.484(6) 0.13(4) Uiso 1 1 d D . . H0AA H 0.209(14) -0.315(11) 0.564(4) 0.14(4) 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 O31 0.151(6) 0.074(3) 0.182(7) 0.023(4) -0.086(5) -0.002(3) N21 0.047(3) 0.038(2) 0.102(4) 0.002(2) 0.005(3) 0.0006(19) N23 0.040(2) 0.050(3) 0.079(3) 0.000(2) -0.009(2) -0.0051(19) C22 0.040(3) 0.050(3) 0.093(5) 0.007(3) -0.003(3) -0.002(2) C30 0.151(6) 0.074(3) 0.182(7) 0.023(4) -0.086(5) -0.002(3) C29 0.033(2) 0.043(3) 0.073(4) 0.006(2) 0.003(2) -0.0011(19) C26 0.072(4) 0.067(4) 0.065(4) 0.001(3) 0.010(3) 0.005(3) C24 0.052(3) 0.042(3) 0.085(4) 0.003(3) 0.003(3) -0.003(2) C27 0.064(4) 0.054(3) 0.074(4) -0.008(3) 0.014(3) 0.000(3) C28 0.040(3) 0.044(3) 0.077(4) 0.000(3) 0.012(2) 0.000(2) C25 0.066(4) 0.050(3) 0.081(4) 0.016(3) 0.010(3) 0.005(3) O11 0.076(3) 0.054(2) 0.043(2) 0.0079(16) -0.0073(18) 0.001(2) N1 0.053(2) 0.044(2) 0.0330(19) -0.0027(16) -0.0026(16) 0.0001(18) N3 0.043(2) 0.044(2) 0.0339(19) -0.0003(16) -0.0046(15) -0.0014(16) C10 0.084(4) 0.040(3) 0.044(3) 0.004(2) -0.012(3) -0.002(3) C9 0.033(2) 0.043(2) 0.038(2) -0.0012(18) -0.0008(17) -0.0036(17) C6 0.055(3) 0.044(3) 0.066(4) 0.006(2) -0.001(3) -0.002(2) C2 0.045(2) 0.040(2) 0.038(2) -0.0018(18) -0.0029(18) 0.0019(19) C8 0.034(2) 0.042(2) 0.038(2) -0.0007(18) -0.0010(17) 0.0005(17) C4 0.057(3) 0.052(3) 0.047(3) -0.010(2) -0.007(2) -0.009(2) C5 0.067(4) 0.043(3) 0.072(4) -0.013(3) -0.006(3) -0.009(3) C7 0.046(3) 0.048(3) 0.045(3) 0.007(2) -0.004(2) 0.000(2) Ru1 0.0368(3) 0.0318(3) 0.0303(3) 0.00020(17) -0.00641(18) -0.00474(18) Cl1 0.0491(7) 0.0580(7) 0.0429(6) 0.0035(5) 0.0033(5) -0.0076(5) Cl3 0.0847(12) 0.0852(12) 0.0697(10) -0.0064(9) -0.0171(9) -0.0132(9) Cl2 0.0733(9) 0.0346(6) 0.0465(7) -0.0010(5) -0.0092(6) -0.0037(5) O0A 0.092(4) 0.108(4) 0.040(2) 0.002(2) -0.014(2) -0.014(3) Cl0 0.0756(10) 0.0520(8) 0.0668(9) -0.0035(7) -0.0141(7) -0.0056(7) O0B 0.075(3) 0.105(4) 0.071(3) 0.004(3) 0.004(3) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O31 C30 1.328(14) . ? O31 H31 0.8200 . ? N21 C22 1.328(9) . ? N21 C28 1.399(8) . ? N21 H21 0.8600 . ? N23 C22 1.343(8) . ? N23 C29 1.391(8) . ? N23 H23 0.8600 . ? C22 C30 1.563(13) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C29 C28 1.378(9) . ? C29 C24 1.391(8) . ? C26 C27 1.381(10) . ? C26 C25 1.390(10) . ? C26 H26 0.9300 . ? C24 C25 1.383(10) . ? C24 H24 0.9300 . ? C27 C28 1.382(10) . ? C27 H27 0.9300 . ? C25 H25 0.9300 . ? O11 C10 1.402(6) . ? O11 H11 0.8200 . ? N1 C2 1.327(6) . ? N1 C8 1.382(6) . ? N1 H1 0.8600 . ? N3 C2 1.334(6) . ? N3 C9 1.382(6) . ? N3 H3 0.8600 . ? C10 C2 1.487(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C9 C8 1.391(6) . ? C9 C4 1.391(7) . ? C6 C7 1.374(8) . ? C6 C5 1.402(9) . ? C6 H6 0.9300 . ? C8 C7 1.399(7) . ? C4 C5 1.382(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 H7 0.9300 . ? Ru1 Cl3 2.282(2) 2_565 ? Ru1 Cl3 2.282(2) . ? Ru1 Cl1 2.3570(14) 2_565 ? Ru1 Cl1 2.3571(14) . ? Ru1 Cl2 2.3790(17) 2_565 ? Ru1 Cl2 2.3790(17) . ? O0A H0AB 0.96(2) . ? O0A H0AA 0.96(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 C30 O31 H31 109.5 . . ? C22 N21 C28 109.3(5) . . ? C22 N21 H21 125.4 . . ? C28 N21 H21 125.4 . . ? C22 N23 C29 108.9(6) . . ? C22 N23 H23 125.6 . . ? C29 N23 H23 125.6 . . ? N21 C22 N23 108.8(6) . . ? N21 C22 C30 128.3(7) . . ? N23 C22 C30 122.4(8) . . ? O31 C30 C22 109.1(11) . . ? O31 C30 H30A 109.9 . . ? C22 C30 H30A 109.9 . . ? O31 C30 H30B 109.9 . . ? C22 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? C28 C29 N23 106.8(5) . . ? C28 C29 C24 121.9(6) . . ? N23 C29 C24 131.4(6) . . ? C27 C26 C25 121.0(7) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C25 C24 C29 115.1(6) . . ? C25 C24 H24 122.5 . . ? C29 C24 H24 122.5 . . ? C28 C27 C26 116.1(6) . . ? C28 C27 H27 121.9 . . ? C26 C27 H27 121.9 . . ? C29 C28 C27 122.7(6) . . ? C29 C28 N21 106.3(6) . . ? C27 C28 N21 131.0(6) . . ? C24 C25 C26 123.2(6) . . ? C24 C25 H25 118.4 . . ? C26 C25 H25 118.4 . . ? C10 O11 H11 109.5 . . ? C2 N1 C8 109.6(4) . . ? C2 N1 H1 125.2 . . ? C8 N1 H1 125.2 . . ? C2 N3 C9 108.8(4) . . ? C2 N3 H3 125.6 . . ? C9 N3 H3 125.6 . . ? O11 C10 C2 111.2(5) . . ? O11 C10 H10A 109.4 . . ? C2 C10 H10A 109.4 . . ? O11 C10 H10B 109.4 . . ? C2 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N3 C9 C8 106.8(4) . . ? N3 C9 C4 131.3(5) . . ? C8 C9 C4 121.9(5) . . ? C7 C6 C5 122.2(5) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? N1 C2 N3 109.0(4) . . ? N1 C2 C10 127.2(5) . . ? N3 C2 C10 123.7(4) . . ? N1 C8 C9 105.8(4) . . ? N1 C8 C7 132.7(5) . . ? C9 C8 C7 121.4(5) . . ? C5 C4 C9 116.6(5) . . ? C5 C4 H4 121.7 . . ? C9 C4 H4 121.7 . . ? C4 C5 C6 121.5(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C6 C7 C8 116.4(5) . . ? C6 C7 H7 121.8 . . ? C8 C7 H7 121.8 . . ? Cl3 Ru1 Cl3 180.0 2_565 . ? Cl3 Ru1 Cl1 90.46(8) 2_565 2_565 ? Cl3 Ru1 Cl1 89.54(8) . 2_565 ? Cl3 Ru1 Cl1 89.54(8) 2_565 . ? Cl3 Ru1 Cl1 90.46(8) . . ? Cl1 Ru1 Cl1 180.0 2_565 . ? Cl3 Ru1 Cl2 89.04(6) 2_565 2_565 ? Cl3 Ru1 Cl2 90.96(6) . 2_565 ? Cl1 Ru1 Cl2 89.42(5) 2_565 2_565 ? Cl1 Ru1 Cl2 90.58(5) . 2_565 ? Cl3 Ru1 Cl2 90.96(6) 2_565 . ? Cl3 Ru1 Cl2 89.04(6) . . ? Cl1 Ru1 Cl2 90.58(5) 2_565 . ? Cl1 Ru1 Cl2 89.42(5) . . ? Cl2 Ru1 Cl2 180.0 2_565 . ? H0AB O0A H0AA 100(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 C28 N21 C22 N23 -1.5(7) . . . . ? C28 N21 C22 C30 -173.0(8) . . . . ? C29 N23 C22 N21 2.0(6) . . . . ? C29 N23 C22 C30 174.1(8) . . . . ? N21 C22 C30 O31 -23.6(14) . . . . ? N23 C22 C30 O31 165.9(8) . . . . ? C22 N23 C29 C28 -1.7(6) . . . . ? C22 N23 C29 C24 177.9(6) . . . . ? C28 C29 C24 C25 0.8(8) . . . . ? N23 C29 C24 C25 -178.8(6) . . . . ? C25 C26 C27 C28 0.1(10) . . . . ? N23 C29 C28 C27 179.5(5) . . . . ? C24 C29 C28 C27 -0.1(9) . . . . ? N23 C29 C28 N21 0.7(6) . . . . ? C24 C29 C28 N21 -178.9(5) . . . . ? C26 C27 C28 C29 -0.3(9) . . . . ? C26 C27 C28 N21 178.1(6) . . . . ? C22 N21 C28 C29 0.4(6) . . . . ? C22 N21 C28 C27 -178.2(6) . . . . ? C29 C24 C25 C26 -1.0(10) . . . . ? C27 C26 C25 C24 0.6(11) . . . . ? C2 N3 C9 C8 -0.2(5) . . . . ? C2 N3 C9 C4 178.8(5) . . . . ? C8 N1 C2 N3 -1.2(6) . . . . ? C8 N1 C2 C10 177.8(5) . . . . ? C9 N3 C2 N1 0.9(6) . . . . ? C9 N3 C2 C10 -178.2(5) . . . . ? O11 C10 C2 N1 173.0(5) . . . . ? O11 C10 C2 N3 -8.2(8) . . . . ? C2 N1 C8 C9 1.1(5) . . . . ? C2 N1 C8 C7 -179.8(5) . . . . ? N3 C9 C8 N1 -0.5(5) . . . . ? C4 C9 C8 N1 -179.6(5) . . . . ? N3 C9 C8 C7 -179.8(4) . . . . ? C4 C9 C8 C7 1.1(7) . . . . ? N3 C9 C4 C5 -178.9(5) . . . . ? C8 C9 C4 C5 -0.1(8) . . . . ? C9 C4 C5 C6 -1.0(9) . . . . ? C7 C6 C5 C4 1.2(10) . . . . ? C5 C6 C7 C8 -0.1(9) . . . . ? N1 C8 C7 C6 180.0(5) . . . . ? C9 C8 C7 C6 -1.0(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O31 H31 Cl3 0.82 1.95 2.545(7) 128.3 2_565 y N23 H23 O0B 0.86 1.91 2.765(9) 169.8 2 y O11 H11 Cl0 0.82 2.21 3.018(5) 167.5 2_656 y N3 H3 O0A 0.86 1.87 2.690(6) 158.4 1_565 y N21 H21 Cl0 0.86 2.21 3.037(6) 161.0 2_656 y N1 H1 Cl2 0.86 2.54 3.301(4) 147.5 . y N1 H1 Cl1 0.86 2.89 3.509(5) 130.3 . y N1 H1 Cl3 0.86 2.91 3.514(5) 129.2 2_565 y O0A H0AB O11 0.96(2) 2.62(6) 3.454(8) 145(8) 1_545 y O0A H0AA Cl0 0.96(2) 2.20(4) 3.134(5) 163(9) . y _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.018 _refine_diff_density_min -1.229 _refine_diff_density_rms 0.127