# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Pankaj K. Pal' 'Michael G. B. Drew' 'Dipankar Datta' _publ_contact_author_name 'Dr Dipankar Datta' _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science Calcutta 700 032 INDIA ; _publ_contact_author_email 'ICDD@MAHENDRA.IACS.RES.IN' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Tuning of intramolecular electron transfer between Ru(II) and disulfide bond ; _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands ; data_(3) _database_code_CSD 183362 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ru(bisox)2(2-thiolatopyridine)]ClO4 _chemical_formula_sum 'C25 H36 Cl N5 O8 Ru S' _chemical_formula_weight 703.17 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' 'S' 'S' 0.1246 0.1234 '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 P21/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 9.983(14) _cell_length_b 11.145(14) _cell_length_c 27.83(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.836(10) _cell_angle_gamma 90.00 _cell_volume 3085(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6325 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.92 _reflns_number_total 3730 _reflns_number_gt 2599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.1844P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3730 _refine_ls_number_parameters 378 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1115 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2379 _refine_ls_wR_factor_gt 0.2148 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.130 _refine_ls_shift/su_mean 0.009 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.40018(6) 0.16027(7) 0.100829(19) 0.0408(4) Uani 1 d . . . S1 S 0.4409(2) 0.1673(2) 0.01610(7) 0.0527(7) Uani 1 d . . . N21 N 0.2423(6) 0.2385(6) 0.0592(2) 0.0427(18) Uani 1 d . . . C22 C 0.1255(8) 0.2920(10) 0.0668(3) 0.057(3) Uani 1 d . . . H22 H 0.0995 0.2972 0.0980 0.069 Uiso 1 calc R . . C23 C 0.0429(10) 0.3398(9) 0.0291(4) 0.071(3) Uani 1 d . . . H23 H -0.0381 0.3760 0.0350 0.085 Uiso 1 calc R . . C24 C 0.0812(11) 0.3333(9) -0.0170(4) 0.070(3) Uani 1 d . . . H24 H 0.0262 0.3654 -0.0424 0.084 Uiso 1 calc R . . C25 C 0.2027(9) 0.2787(10) -0.0257(3) 0.063(3) Uani 1 d . . . H25 H 0.2292 0.2723 -0.0569 0.076 Uiso 1 calc R . . C26 C 0.2833(7) 0.2339(9) 0.0138(3) 0.046(2) Uani 1 d . . . N31 N 0.3339(6) -0.0181(7) 0.0900(2) 0.0442(19) Uani 1 d . . . C35 C 0.4194(8) -0.0985(11) 0.1050(3) 0.048(2) Uani 1 d . . . O34 O 0.3933(6) -0.2191(8) 0.1013(2) 0.078(2) Uani 1 d . . . C32 C 0.2137(8) -0.0872(10) 0.0672(3) 0.052(3) Uani 1 d . . . C33 C 0.2544(11) -0.2164(12) 0.0788(5) 0.099(4) Uani 1 d . . . H34A H 0.1940 -0.2508 0.1006 0.119 Uiso 1 calc R . . H34B H 0.2481 -0.2637 0.0494 0.119 Uiso 1 calc R . . C321 C 0.2027(10) -0.0648(11) 0.0128(3) 0.077(3) Uani 1 d . . . H32A H 0.1782 0.0173 0.0065 0.093 Uiso 1 calc R . . H32B H 0.1354 -0.1166 -0.0026 0.093 Uiso 1 calc R . . H32C H 0.2878 -0.0809 0.0004 0.093 Uiso 1 calc R . . C322 C 0.0866(9) -0.0522(11) 0.0886(4) 0.073(3) Uani 1 d . . . H32D H 0.0959 -0.0672 0.1227 0.088 Uiso 1 calc R . . H32E H 0.0131 -0.0987 0.0739 0.088 Uiso 1 calc R . . H32F H 0.0693 0.0315 0.0829 0.088 Uiso 1 calc R . . C36 C 0.5490(9) -0.0514(12) 0.1284(3) 0.056(3) Uani 1 d . . . N40 N 0.5660(6) 0.0615(9) 0.1308(2) 0.049(2) Uani 1 d . . . C39 C 0.7084(8) 0.0787(10) 0.1536(3) 0.054(3) Uani 1 d . . . C391 C 0.7067(12) 0.1610(16) 0.1960(5) 0.151(9) Uani 1 d . . . H39A H 0.6751 0.2387 0.1853 0.181 Uiso 1 calc R . . H39B H 0.7959 0.1681 0.2115 0.181 Uiso 1 calc R . . H39C H 0.6479 0.1290 0.2184 0.181 Uiso 1 calc R . . C392 C 0.7878(10) 0.1272(15) 0.1146(5) 0.119(6) Uani 1 d . . . H39D H 0.7279 0.1475 0.0870 0.142 Uiso 1 calc R . . H39E H 0.8505 0.0675 0.1057 0.142 Uiso 1 calc R . . H39F H 0.8358 0.1976 0.1261 0.142 Uiso 1 calc R . . C38 C 0.7501(10) -0.0487(11) 0.1673(5) 0.093(4) Uani 1 d . . . H38A H 0.8367 -0.0669 0.1557 0.111 Uiso 1 calc R . . H38B H 0.7576 -0.0576 0.2021 0.111 Uiso 1 calc R . . O37 O 0.6472(6) -0.1306(7) 0.1455(3) 0.072(2) Uani 1 d . . . N51 N 0.4749(7) 0.3335(6) 0.1183(2) 0.044(2) Uani 1 d . . . C52 C 0.5322(8) 0.4417(9) 0.0940(3) 0.050(2) Uani 1 d . . . C521 C 0.4201(10) 0.4959(9) 0.0600(3) 0.062(3) Uani 1 d . . . H52A H 0.4532 0.5659 0.0448 0.075 Uiso 1 calc R . . H52B H 0.3460 0.5179 0.0781 0.075 Uiso 1 calc R . . H52C H 0.3906 0.4381 0.0358 0.075 Uiso 1 calc R . . C522 C 0.6563(9) 0.4122(10) 0.0679(3) 0.068(3) Uani 1 d . . . H52D H 0.7248 0.3796 0.0905 0.082 Uiso 1 calc R . . H52E H 0.6891 0.4839 0.0539 0.082 Uiso 1 calc R . . H52F H 0.6332 0.3544 0.0430 0.082 Uiso 1 calc R . . C53 C 0.5712(9) 0.5268(10) 0.1369(3) 0.062(3) Uani 1 d . . . H53A H 0.6670 0.5237 0.1461 0.074 Uiso 1 calc R . . H53B H 0.5458 0.6090 0.1291 0.074 Uiso 1 calc R . . O54 O 0.4931(7) 0.4790(7) 0.1758(2) 0.066(2) Uani 1 d . . . C55 C 0.4504(9) 0.3709(10) 0.1611(3) 0.052(3) Uani 1 d . . . C56 C 0.3841(8) 0.2879(11) 0.1909(3) 0.053(3) Uani 1 d . . . O57 O 0.3668(7) 0.3137(7) 0.2371(2) 0.066(2) Uani 1 d . . . C58 C 0.3190(10) 0.1992(11) 0.2550(3) 0.070(3) Uani 1 d . . . H58A H 0.2462 0.2125 0.2754 0.084 Uiso 1 calc R . . H58B H 0.3913 0.1580 0.2738 0.084 Uiso 1 calc R . . C59 C 0.2695(8) 0.1236(10) 0.2104(3) 0.052(3) Uani 1 d . . . N60 N 0.3443(7) 0.1856(8) 0.1734(2) 0.046(2) Uani 1 d . . . C591 C 0.1224(9) 0.1458(10) 0.1979(3) 0.069(3) Uani 1 d . . . H59A H 0.1054 0.2306 0.1977 0.083 Uiso 1 calc R . . H59B H 0.0715 0.1081 0.2215 0.083 Uiso 1 calc R . . H59C H 0.0962 0.1130 0.1667 0.083 Uiso 1 calc R . . C592 C 0.3039(10) -0.0050(10) 0.2159(3) 0.067(3) Uani 1 d . . . H59D H 0.2640 -0.0369 0.2434 0.080 Uiso 1 calc R . . H59E H 0.3998 -0.0138 0.2205 0.080 Uiso 1 calc R . . H59F H 0.2703 -0.0477 0.1875 0.080 Uiso 1 calc R . . Cl2 Cl 0.0164(4) 0.5459(5) 0.16511(11) 0.1092(14) Uani 1 d . . . O21 O 0.077(2) 0.566(4) 0.2047(7) 0.410(19) Uani 1 d . . . O22 O -0.061(3) 0.641(2) 0.1594(13) 0.368(18) Uani 1 d . . . O23 O -0.068(2) 0.457(3) 0.1702(11) 0.343(16) Uani 1 d . . . O24 O 0.088(3) 0.5440(18) 0.1301(8) 0.333(14) Uani 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 0.0382(5) 0.0468(8) 0.0371(4) 0.0010(3) 0.0015(2) 0.0042(3) S1 0.0589(14) 0.060(2) 0.0401(11) -0.0017(10) 0.0110(9) 0.0050(12) N21 0.046(4) 0.034(5) 0.048(4) 0.003(3) 0.003(3) 0.005(4) C22 0.047(5) 0.065(8) 0.059(5) 0.001(5) 0.002(4) 0.018(5) C23 0.050(6) 0.059(9) 0.100(8) 0.001(6) -0.017(5) 0.014(5) C24 0.086(8) 0.059(9) 0.058(6) 0.012(5) -0.032(5) -0.013(6) C25 0.065(6) 0.069(9) 0.054(5) 0.000(5) -0.010(4) -0.004(6) C26 0.044(4) 0.050(7) 0.046(4) -0.008(4) 0.005(3) -0.005(4) N31 0.035(4) 0.049(6) 0.049(4) -0.004(4) 0.003(3) -0.002(4) C35 0.039(5) 0.043(8) 0.064(5) -0.003(5) 0.013(4) 0.009(5) O34 0.075(5) 0.055(7) 0.103(6) -0.003(4) -0.006(4) 0.014(4) C32 0.046(5) 0.045(8) 0.065(5) -0.004(5) -0.002(4) 0.000(5) C33 0.069(8) 0.060(10) 0.162(12) 0.001(9) -0.027(7) -0.009(7) C321 0.077(7) 0.085(10) 0.071(6) -0.018(6) 0.007(5) -0.024(6) C322 0.041(5) 0.089(10) 0.092(7) -0.034(6) 0.017(4) -0.021(6) C36 0.044(5) 0.065(9) 0.059(5) 0.011(5) 0.002(4) 0.023(6) N40 0.042(4) 0.055(7) 0.048(4) 0.006(4) -0.005(3) 0.010(5) C39 0.038(5) 0.057(8) 0.064(5) 0.001(5) -0.010(4) 0.001(5) C391 0.061(8) 0.27(3) 0.108(10) -0.087(12) -0.046(7) 0.041(9) C392 0.044(7) 0.156(15) 0.153(12) 0.080(11) -0.011(6) -0.043(8) C38 0.045(6) 0.086(11) 0.140(10) 0.042(8) -0.026(6) -0.005(6) O37 0.055(4) 0.065(6) 0.094(5) 0.020(4) -0.005(3) 0.014(4) N51 0.048(4) 0.046(6) 0.037(3) 0.006(3) -0.002(3) 0.001(4) C52 0.052(5) 0.051(7) 0.045(4) 0.001(4) 0.002(3) 0.004(5) C521 0.087(7) 0.048(7) 0.050(5) 0.009(4) -0.009(4) -0.002(6) C522 0.070(6) 0.055(9) 0.080(6) 0.010(6) 0.008(5) -0.012(6) C53 0.053(6) 0.070(9) 0.060(5) 0.012(5) -0.010(4) -0.010(5) O54 0.087(5) 0.063(6) 0.047(3) -0.012(3) -0.001(3) -0.014(4) C55 0.062(6) 0.052(8) 0.040(4) -0.002(5) -0.007(4) 0.013(5) C56 0.060(5) 0.067(8) 0.031(4) 0.003(5) 0.003(3) 0.003(6) O57 0.086(4) 0.075(6) 0.038(3) -0.005(3) 0.007(3) -0.006(4) C58 0.070(6) 0.098(10) 0.042(5) 0.003(5) 0.010(4) -0.007(6) C59 0.054(5) 0.066(8) 0.038(4) -0.006(4) 0.014(3) 0.004(5) N60 0.044(4) 0.050(6) 0.044(4) -0.005(4) 0.008(3) -0.001(4) C591 0.059(6) 0.078(9) 0.073(6) 0.004(6) 0.029(4) -0.001(5) C592 0.078(7) 0.073(9) 0.049(5) 0.012(5) 0.009(4) -0.008(6) Cl2 0.106(2) 0.155(5) 0.0680(18) -0.008(2) 0.0175(16) -0.008(3) O21 0.25(2) 0.83(6) 0.137(13) -0.12(2) -0.057(14) -0.05(3) O22 0.41(4) 0.20(2) 0.52(5) 0.04(3) 0.19(3) 0.15(3) O23 0.179(17) 0.36(3) 0.48(4) 0.21(3) -0.012(18) -0.082(19) O24 0.54(4) 0.24(2) 0.257(19) -0.091(15) 0.28(2) -0.06(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 N21 2.068(6) . ? Ru1 N40 2.101(7) . ? Ru1 N31 2.109(8) . ? Ru1 N51 2.112(7) . ? Ru1 N60 2.159(7) . ? Ru1 S1 2.428(4) . ? S1 C26 1.736(8) . ? N21 C22 1.342(10) . ? N21 C26 1.362(10) . ? C22 C23 1.385(13) . ? C23 C24 1.369(16) . ? C24 C25 1.397(14) . ? C25 C26 1.399(11) . ? N31 C35 1.283(12) . ? N31 C32 1.520(11) . ? C35 O34 1.372(14) . ? C35 C36 1.494(13) . ? O34 C33 1.473(12) . ? C32 C322 1.498(12) . ? C32 C33 1.524(16) . ? C32 C321 1.528(13) . ? C36 N40 1.270(12) . ? C36 O37 1.374(11) . ? N40 C39 1.519(10) . ? C39 C392 1.497(14) . ? C39 C391 1.497(15) . ? C39 C38 1.520(15) . ? C38 O37 1.467(13) . ? N51 C55 1.304(10) . ? N51 C52 1.518(11) . ? C52 C522 1.523(12) . ? C52 C521 1.528(12) . ? C52 C53 1.549(13) . ? C53 O54 1.485(11) . ? O54 C55 1.331(11) . ? C55 C56 1.440(13) . ? C56 N60 1.288(12) . ? C56 O57 1.344(10) . ? O57 C58 1.465(12) . ? C58 C59 1.546(13) . ? C59 C592 1.479(14) . ? C59 N60 1.492(11) . ? C59 C591 1.500(12) . ? Cl2 O21 1.232(15) . ? Cl2 O24 1.255(15) . ? Cl2 O22 1.31(2) . ? Cl2 O23 1.32(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 N21 Ru1 N40 168.8(3) . . ? N21 Ru1 N31 95.9(3) . . ? N40 Ru1 N31 77.9(3) . . ? N21 Ru1 N51 88.9(3) . . ? N40 Ru1 N51 97.8(3) . . ? N31 Ru1 N51 174.4(2) . . ? N21 Ru1 N60 102.9(3) . . ? N40 Ru1 N60 87.4(3) . . ? N31 Ru1 N60 98.9(3) . . ? N51 Ru1 N60 77.2(3) . . ? N21 Ru1 S1 67.95(19) . . ? N40 Ru1 S1 102.2(2) . . ? N31 Ru1 S1 88.15(18) . . ? N51 Ru1 S1 96.28(18) . . ? N60 Ru1 S1 169.2(2) . . ? C26 S1 Ru1 79.9(3) . . ? C22 N21 C26 119.7(7) . . ? C22 N21 Ru1 137.0(5) . . ? C26 N21 Ru1 103.2(5) . . ? N21 C22 C23 121.5(9) . . ? C24 C23 C22 119.5(10) . . ? C23 C24 C25 120.1(8) . . ? C24 C25 C26 118.0(8) . . ? N21 C26 C25 121.2(8) . . ? N21 C26 S1 108.9(6) . . ? C25 C26 S1 129.9(7) . . ? C35 N31 C32 105.2(8) . . ? C35 N31 Ru1 114.8(6) . . ? C32 N31 Ru1 139.9(6) . . ? N31 C35 O34 122.9(8) . . ? N31 C35 C36 115.1(10) . . ? O34 C35 C36 122.0(9) . . ? C35 O34 C33 100.2(8) . . ? C322 C32 N31 111.6(7) . . ? C322 C32 C33 112.4(9) . . ? N31 C32 C33 101.7(7) . . ? C322 C32 C321 111.1(8) . . ? N31 C32 C321 108.6(7) . . ? C33 C32 C321 111.1(9) . . ? O34 C33 C32 109.6(9) . . ? N40 C36 O37 122.0(9) . . ? N40 C36 C35 118.6(8) . . ? O37 C36 C35 119.5(10) . . ? C36 N40 C39 105.3(8) . . ? C36 N40 Ru1 113.6(6) . . ? C39 N40 Ru1 141.0(7) . . ? C392 C39 C391 113.2(12) . . ? C392 C39 N40 106.1(7) . . ? C391 C39 N40 109.5(7) . . ? C392 C39 C38 111.7(10) . . ? C391 C39 C38 113.2(11) . . ? N40 C39 C38 102.3(8) . . ? O37 C38 C39 108.0(7) . . ? C36 O37 C38 101.5(8) . . ? C55 N51 C52 105.1(7) . . ? C55 N51 Ru1 114.4(6) . . ? C52 N51 Ru1 139.7(5) . . ? N51 C52 C522 113.1(8) . . ? N51 C52 C521 107.8(7) . . ? C522 C52 C521 112.0(7) . . ? N51 C52 C53 102.8(6) . . ? C522 C52 C53 109.7(7) . . ? C521 C52 C53 111.0(8) . . ? O54 C53 C52 103.3(7) . . ? C55 O54 C53 105.9(7) . . ? N51 C55 O54 119.4(8) . . ? N51 C55 C56 116.8(9) . . ? O54 C55 C56 123.7(8) . . ? N60 C56 O57 119.4(8) . . ? N60 C56 C55 119.6(7) . . ? O57 C56 C55 121.0(9) . . ? C56 O57 C58 102.2(7) . . ? O57 C58 C59 107.0(7) . . ? C592 C59 N60 113.2(7) . . ? C592 C59 C591 113.5(9) . . ? N60 C59 C591 107.5(7) . . ? C592 C59 C58 112.9(8) . . ? N60 C59 C58 99.0(8) . . ? C591 C59 C58 109.7(8) . . ? C56 N60 C59 107.8(7) . . ? C56 N60 Ru1 111.9(5) . . ? C59 N60 Ru1 140.3(6) . . ? O21 Cl2 O24 115.4(19) . . ? O21 Cl2 O22 102(2) . . ? O24 Cl2 O22 106.7(17) . . ? O21 Cl2 O23 108(2) . . ? O24 Cl2 O23 118.6(18) . . ? O22 Cl2 O23 104.2(19) . . ? _refine_diff_density_max 1.485 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.148 #====END data_(1) _database_code_CSD 183363 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ru(bpy)2(DTDP)](ClO4)2.H2O _chemical_formula_sum 'C30 H26 Cl2 N6 O9 Ru S2' _chemical_formula_weight 850.66 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' 'S' 'S' 0.1246 0.1234 '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 10.046(14) _cell_length_b 12.988(17) _cell_length_c 15.224(17) _cell_angle_alpha 68.989(10) _cell_angle_beta 75.212(10) _cell_angle_gamma 68.217(10) _cell_volume 1705(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 0.801 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5797 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 26.06 _reflns_number_total 5797 _reflns_number_gt 3101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.1830P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5797 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1647 _refine_ls_R_factor_gt 0.0887 _refine_ls_wR_factor_ref 0.2837 _refine_ls_wR_factor_gt 0.2518 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.005 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.76969(8) 0.66865(6) 0.75180(5) 0.0601(3) Uani 1 d . . . N11 N 0.8488(8) 0.5242(7) 0.7032(5) 0.0628(19) Uani 1 d . . . C12 C 0.9403(11) 0.4194(9) 0.7446(9) 0.078(3) Uani 1 d . . . H12 H 0.9658 0.4075 0.8028 0.094 Uiso 1 calc R . . C13 C 0.9978(13) 0.3287(10) 0.7034(10) 0.086(3) Uani 1 d . . . H13 H 1.0600 0.2578 0.7336 0.104 Uiso 1 calc R . . C14 C 0.9601(14) 0.3470(12) 0.6176(11) 0.095(4) Uani 1 d . . . H14 H 1.0005 0.2890 0.5877 0.114 Uiso 1 calc R . . C15 C 0.8626(14) 0.4507(11) 0.5746(9) 0.086(3) Uani 1 d . . . H15 H 0.8322 0.4618 0.5182 0.103 Uiso 1 calc R . . C16 C 0.8103(11) 0.5405(10) 0.6204(8) 0.073(3) Uani 1 d . . . C17 C 0.7075(11) 0.6499(9) 0.5835(7) 0.073(3) Uani 1 d . . . C18 C 0.6503(14) 0.6865(11) 0.4952(8) 0.087(3) Uani 1 d . . . H18 H 0.6841 0.6389 0.4557 0.104 Uiso 1 calc R . . C19 C 0.5451(14) 0.7927(13) 0.4700(8) 0.093(4) Uani 1 d . . . H19 H 0.5114 0.8185 0.4120 0.111 Uiso 1 calc R . . C20 C 0.4897(13) 0.8611(11) 0.5314(8) 0.082(3) Uani 1 d . . . H20 H 0.4149 0.9305 0.5169 0.099 Uiso 1 calc R . . C21 C 0.5486(11) 0.8236(9) 0.6147(8) 0.072(3) Uani 1 d . . . H21 H 0.5111 0.8690 0.6561 0.087 Uiso 1 calc R . . N22 N 0.6548(8) 0.7270(7) 0.6378(5) 0.0590(19) Uani 1 d . . . N31 N 0.9451(7) 0.7203(6) 0.6640(5) 0.0590(18) Uani 1 d . . . C32 C 0.9296(12) 0.8046(9) 0.5790(7) 0.070(3) Uani 1 d . . . H32 H 0.8364 0.8405 0.5631 0.084 Uiso 1 calc R . . C33 C 1.0362(16) 0.8410(12) 0.5158(8) 0.099(4) Uani 1 d . . . H33 H 1.0153 0.9027 0.4611 0.118 Uiso 1 calc R . . C34 C 1.1800(16) 0.7831(15) 0.5348(9) 0.109(5) Uani 1 d . . . H34 H 1.2572 0.8010 0.4906 0.131 Uiso 1 calc R . . C35 C 1.2039(12) 0.6947(12) 0.6252(9) 0.097(4) Uani 1 d . . . H35 H 1.2966 0.6560 0.6416 0.117 Uiso 1 calc R . . C44 C 0.9761(10) 0.7594(9) 0.9092(7) 0.070(3) Uani 1 d . . . H44 H 1.0425 0.7659 0.8539 0.084 Uiso 1 calc R . . S37 S 1.1182(3) 0.5633(2) 0.7936(2) 0.0772(8) Uani 1 d . . . S38 S 0.9137(3) 0.5842(2) 0.87163(17) 0.0623(6) Uani 1 d . . . C39 C 0.8968(11) 0.6819(8) 0.9371(7) 0.066(2) Uani 1 d . . . N40 N 0.8025(9) 0.6675(7) 1.0133(6) 0.070(2) Uani 1 d . . . C41 C 0.7767(12) 0.7346(11) 1.0702(8) 0.085(3) Uani 1 d . . . H41 H 0.7077 0.7278 1.1241 0.102 Uiso 1 calc R . . C42 C 0.8524(13) 0.8141(10) 1.0492(8) 0.079(3) Uani 1 d . . . H42 H 0.8359 0.8579 1.0898 0.095 Uiso 1 calc R . . C43 C 0.9500(12) 0.8263(10) 0.9690(9) 0.081(3) Uani 1 d . . . H43 H 0.9996 0.8797 0.9540 0.097 Uiso 1 calc R . . C36 C 1.0859(11) 0.6699(9) 0.6854(7) 0.070(3) Uani 1 d . . . N61 N 0.6710(7) 0.8171(6) 0.7953(5) 0.0561(18) Uani 1 d . . . C62 C 0.7199(12) 0.9074(9) 0.7698(9) 0.081(3) Uani 1 d . . . H62 H 0.8055 0.9085 0.7282 0.097 Uiso 1 calc R . . C63 C 0.6385(15) 1.0034(10) 0.8076(11) 0.100(4) Uani 1 d . . . H63 H 0.6696 1.0685 0.7866 0.120 Uiso 1 calc R . . C64 C 0.5259(16) 1.0026(12) 0.8684(11) 0.105(4) Uani 1 d . . . H64 H 0.4813 1.0627 0.8959 0.126 Uiso 1 calc R . . C65 C 0.4689(12) 0.9111(10) 0.8942(9) 0.086(3) Uani 1 d . . . H65 H 0.3827 0.9124 0.9356 0.103 Uiso 1 calc R . . C66 C 0.5423(9) 0.8181(8) 0.8574(7) 0.066(2) Uani 1 d . . . C67 C 0.4976(10) 0.7143(8) 0.8805(7) 0.064(2) Uani 1 d . . . C68 C 0.3707(11) 0.7017(10) 0.9358(7) 0.078(3) Uani 1 d . . . H68 H 0.3114 0.7569 0.9663 0.093 Uiso 1 calc R . . C69 C 0.3313(11) 0.6061(11) 0.9461(9) 0.086(4) Uani 1 d . . . H69 H 0.2449 0.5976 0.9834 0.104 Uiso 1 calc R . . C70 C 0.4161(12) 0.5260(10) 0.9029(8) 0.076(3) Uani 1 d . . . H70 H 0.3876 0.4633 0.9081 0.091 Uiso 1 calc R . . C71 C 0.5487(12) 0.5379(9) 0.8496(7) 0.071(3) Uani 1 d . . . H71 H 0.6109 0.4806 0.8221 0.086 Uiso 1 calc R . . N72 N 0.5867(8) 0.6318(6) 0.8378(5) 0.0581(18) Uani 1 d . . . Cl6 Cl 1.1471(3) 0.9914(2) 0.7248(2) 0.0832(8) Uani 1 d . . . O61 O 1.1357(18) 1.0270(13) 0.8036(11) 0.186(6) Uani 1 d . . . O62 O 1.0057(11) 1.0086(12) 0.7148(9) 0.172(6) Uani 1 d . . . O64 O 1.2095(10) 1.0581(8) 0.6393(8) 0.130(4) Uani 1 d . . . O65 O 1.2266(11) 0.8739(8) 0.7472(8) 0.132(4) Uani 1 d . . . Cl7 Cl 1.5206(3) 0.3516(3) 0.7018(2) 0.0907(9) Uani 1 d . . . O71 O 1.5165(14) 0.4701(9) 0.6671(10) 0.155(5) Uani 1 d . . . O72 O 1.3893(12) 0.3372(13) 0.7016(8) 0.150(5) Uani 1 d . . . O73 O 1.5551(12) 0.3036(10) 0.7986(8) 0.129(3) Uani 1 d . . . O74 O 1.6270(13) 0.2908(11) 0.6441(10) 0.159(5) Uani 1 d . . . O100 O 1.8057(11) 0.1529(10) 0.8965(7) 0.131(3) Uani 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 0.0577(5) 0.0504(5) 0.0675(5) -0.0144(4) -0.0108(3) -0.0130(3) N11 0.071(5) 0.065(5) 0.059(5) -0.018(4) -0.011(4) -0.027(4) C12 0.068(6) 0.062(7) 0.107(8) -0.020(6) -0.032(6) -0.014(5) C13 0.092(8) 0.061(7) 0.110(10) -0.043(7) -0.007(7) -0.017(6) C14 0.089(8) 0.083(9) 0.121(11) -0.057(8) 0.013(7) -0.027(7) C15 0.105(9) 0.085(8) 0.077(7) -0.032(6) -0.011(6) -0.034(7) C16 0.058(6) 0.081(8) 0.085(7) -0.031(6) 0.004(5) -0.030(5) C17 0.070(6) 0.073(7) 0.076(7) -0.011(6) -0.004(5) -0.038(5) C18 0.095(8) 0.100(9) 0.077(7) -0.029(7) -0.026(6) -0.030(7) C19 0.096(9) 0.128(11) 0.065(7) -0.010(7) -0.019(6) -0.060(9) C20 0.079(7) 0.092(8) 0.078(7) -0.010(6) -0.026(6) -0.032(6) C21 0.065(6) 0.054(6) 0.084(7) -0.015(5) -0.018(5) -0.003(5) N22 0.065(5) 0.066(5) 0.058(4) -0.022(4) 0.003(3) -0.037(4) N31 0.045(4) 0.054(4) 0.070(5) -0.019(4) -0.008(3) -0.005(3) C32 0.080(7) 0.075(7) 0.054(5) -0.007(5) -0.008(5) -0.035(5) C33 0.127(12) 0.112(10) 0.059(6) -0.002(6) -0.013(6) -0.062(9) C34 0.099(10) 0.168(14) 0.066(7) -0.031(8) 0.016(6) -0.069(9) C35 0.062(7) 0.126(11) 0.092(9) -0.035(8) 0.002(6) -0.023(7) C44 0.060(6) 0.078(7) 0.067(6) -0.008(5) -0.007(4) -0.031(5) S37 0.0579(14) 0.0750(18) 0.0813(17) -0.0200(14) -0.0140(12) -0.0014(12) S38 0.0601(13) 0.0540(14) 0.0659(14) -0.0112(11) -0.0141(10) -0.0127(11) C39 0.068(6) 0.056(6) 0.060(6) -0.006(4) -0.014(5) -0.010(5) N40 0.078(5) 0.056(5) 0.067(5) -0.012(4) -0.009(4) -0.016(4) C41 0.079(7) 0.099(9) 0.067(7) -0.033(6) 0.001(5) -0.016(6) C42 0.082(7) 0.072(7) 0.083(7) -0.032(6) -0.023(6) -0.008(6) C43 0.071(7) 0.082(8) 0.100(8) -0.037(7) -0.015(6) -0.023(6) C36 0.065(6) 0.073(7) 0.069(6) -0.025(5) -0.007(5) -0.015(5) N61 0.047(4) 0.039(4) 0.073(5) -0.011(3) -0.014(3) -0.004(3) C62 0.075(7) 0.059(7) 0.099(8) -0.022(6) -0.034(6) 0.004(5) C63 0.106(10) 0.054(7) 0.144(12) -0.041(7) 0.005(9) -0.033(6) C64 0.107(10) 0.087(9) 0.127(11) -0.067(8) 0.010(8) -0.021(8) C65 0.067(7) 0.072(7) 0.120(10) -0.044(7) -0.008(6) -0.010(5) C66 0.043(5) 0.064(6) 0.083(7) -0.025(5) -0.015(4) -0.001(4) C67 0.068(6) 0.048(5) 0.067(6) -0.005(5) -0.018(5) -0.014(5) C68 0.058(6) 0.084(8) 0.075(7) -0.012(6) -0.001(5) -0.021(5) C69 0.046(6) 0.104(9) 0.096(8) 0.000(7) -0.019(5) -0.030(6) C70 0.076(7) 0.070(7) 0.076(7) 0.002(6) -0.022(5) -0.030(6) C71 0.091(8) 0.075(7) 0.062(6) -0.015(5) -0.014(5) -0.043(6) N72 0.059(4) 0.054(5) 0.058(4) -0.013(4) -0.018(3) -0.010(4) Cl6 0.0809(19) 0.0655(17) 0.0875(19) -0.0110(14) -0.0133(14) -0.0155(14) O61 0.231(17) 0.177(12) 0.185(13) -0.108(11) -0.001(11) -0.066(11) O62 0.091(7) 0.208(13) 0.150(10) 0.044(9) -0.041(6) -0.050(8) O64 0.097(6) 0.106(7) 0.137(8) 0.012(6) 0.015(6) -0.043(5) O65 0.123(8) 0.062(5) 0.152(9) -0.005(5) 0.006(6) -0.006(5) Cl7 0.089(2) 0.090(2) 0.097(2) -0.0377(18) -0.0004(15) -0.0305(16) O71 0.169(11) 0.078(7) 0.195(12) -0.005(7) -0.053(9) -0.028(7) O72 0.119(8) 0.259(15) 0.132(8) -0.094(9) 0.026(6) -0.119(9) O73 0.134(9) 0.145(9) 0.121(8) -0.042(7) -0.029(6) -0.047(7) O74 0.128(9) 0.183(11) 0.194(12) -0.130(10) 0.057(8) -0.057(8) O100 0.104(7) 0.165(10) 0.113(7) -0.046(7) -0.002(5) -0.031(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 N11 2.070(8) . ? Ru1 N72 2.073(8) . ? Ru1 N61 2.074(8) . ? Ru1 N22 2.085(8) . ? Ru1 N31 2.092(8) . ? Ru1 S38 2.315(3) . ? N11 C16 1.334(13) . ? N11 C12 1.359(12) . ? C12 C13 1.398(16) . ? C13 C14 1.367(19) . ? C14 C15 1.385(18) . ? C15 C16 1.436(16) . ? C16 C17 1.427(15) . ? C17 N22 1.395(13) . ? C17 C18 1.448(15) . ? C18 C19 1.383(17) . ? C19 C20 1.390(17) . ? C20 C21 1.387(15) . ? C21 N22 1.310(12) . ? N31 C32 1.362(11) . ? N31 C36 1.389(12) . ? C32 C33 1.349(15) . ? C33 C34 1.410(19) . ? C34 C35 1.449(18) . ? C35 C36 1.366(14) . ? C44 C43 1.388(15) . ? C44 C39 1.395(14) . ? S37 C36 1.745(10) . ? S37 S38 2.068(4) . ? S38 C39 1.814(11) . ? C39 N40 1.300(13) . ? N40 C41 1.356(14) . ? C41 C42 1.403(16) . ? C42 C43 1.358(16) . ? N61 C62 1.331(13) . ? N61 C66 1.392(12) . ? C62 C63 1.439(16) . ? C63 C64 1.266(17) . ? C64 C65 1.396(17) . ? C65 C66 1.389(15) . ? C66 C67 1.474(13) . ? C67 N72 1.364(12) . ? C67 C68 1.367(14) . ? C68 C69 1.384(16) . ? C69 C70 1.338(17) . ? C70 C71 1.402(15) . ? C71 N72 1.349(12) . ? Cl6 O62 1.394(11) . ? Cl6 O65 1.395(9) . ? Cl6 O61 1.397(14) . ? Cl6 O64 1.420(9) . ? Cl7 O74 1.389(10) . ? Cl7 O72 1.400(10) . ? Cl7 O71 1.425(10) . ? Cl7 O73 1.457(11) . ? 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 N11 Ru1 N72 97.2(3) . . ? N11 Ru1 N61 174.2(3) . . ? N72 Ru1 N61 79.6(3) . . ? N11 Ru1 N22 79.3(3) . . ? N72 Ru1 N22 86.6(3) . . ? N61 Ru1 N22 95.6(3) . . ? N11 Ru1 N31 87.1(3) . . ? N72 Ru1 N31 175.3(3) . . ? N61 Ru1 N31 96.0(3) . . ? N22 Ru1 N31 92.2(3) . . ? N11 Ru1 S38 93.7(2) . . ? N72 Ru1 S38 95.4(2) . . ? N61 Ru1 S38 91.4(2) . . ? N22 Ru1 S38 172.9(2) . . ? N31 Ru1 S38 86.3(2) . . ? C16 N11 C12 118.4(9) . . ? C16 N11 Ru1 115.1(7) . . ? C12 N11 Ru1 126.4(7) . . ? N11 C12 C13 122.9(11) . . ? C14 C13 C12 118.2(12) . . ? C13 C14 C15 121.0(12) . . ? C14 C15 C16 117.5(11) . . ? N11 C16 C17 115.7(10) . . ? N11 C16 C15 121.9(10) . . ? C17 C16 C15 122.3(11) . . ? N22 C17 C16 117.5(9) . . ? N22 C17 C18 117.1(10) . . ? C16 C17 C18 125.4(11) . . ? C19 C18 C17 119.5(12) . . ? C18 C19 C20 120.1(10) . . ? C21 C20 C19 118.5(11) . . ? N22 C21 C20 122.9(11) . . ? C21 N22 C17 121.6(9) . . ? C21 N22 Ru1 127.3(7) . . ? C17 N22 Ru1 111.2(6) . . ? C32 N31 C36 114.8(8) . . ? C32 N31 Ru1 121.8(6) . . ? C36 N31 Ru1 123.4(6) . . ? C33 C32 N31 126.5(10) . . ? C32 C33 C34 118.2(11) . . ? C33 C34 C35 118.1(10) . . ? C36 C35 C34 117.9(11) . . ? C43 C44 C39 116.0(9) . . ? C36 S37 S38 102.9(4) . . ? C39 S38 S37 104.8(3) . . ? C39 S38 Ru1 113.3(3) . . ? S37 S38 Ru1 101.19(15) . . ? N40 C39 C44 125.7(10) . . ? N40 C39 S38 110.2(8) . . ? C44 C39 S38 124.1(8) . . ? C39 N40 C41 117.6(9) . . ? N40 C41 C42 121.1(10) . . ? C43 C42 C41 119.4(11) . . ? C42 C43 C44 120.2(11) . . ? C35 C36 N31 124.3(10) . . ? C35 C36 S37 116.8(8) . . ? N31 C36 S37 118.9(7) . . ? C62 N61 C66 119.2(8) . . ? C62 N61 Ru1 126.2(7) . . ? C66 N61 Ru1 114.6(6) . . ? N61 C62 C63 119.1(11) . . ? C64 C63 C62 122.4(11) . . ? C63 C64 C65 119.9(12) . . ? C66 C65 C64 119.3(11) . . ? C65 C66 N61 120.0(9) . . ? C65 C66 C67 125.3(9) . . ? N61 C66 C67 114.8(8) . . ? N72 C67 C68 120.3(9) . . ? N72 C67 C66 115.9(8) . . ? C68 C67 C66 123.6(10) . . ? C67 C68 C69 119.4(11) . . ? C70 C69 C68 120.8(11) . . ? C69 C70 C71 118.9(11) . . ? N72 C71 C70 120.6(11) . . ? C71 N72 C67 119.8(9) . . ? C71 N72 Ru1 125.0(7) . . ? C67 N72 Ru1 115.1(6) . . ? O62 Cl6 O65 111.1(8) . . ? O62 Cl6 O61 105.8(10) . . ? O65 Cl6 O61 106.5(9) . . ? O62 Cl6 O64 107.9(7) . . ? O65 Cl6 O64 112.4(6) . . ? O61 Cl6 O64 113.0(9) . . ? O74 Cl7 O72 107.8(8) . . ? O74 Cl7 O71 109.0(9) . . ? O72 Cl7 O71 112.8(8) . . ? O74 Cl7 O73 109.5(8) . . ? O72 Cl7 O73 108.8(7) . . ? O71 Cl7 O73 109.0(8) . . ? _refine_diff_density_max 1.052 _refine_diff_density_min -1.146 _refine_diff_density_rms 0.139 data_(2) _database_code_CSD 183364 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ru(phen)2(DTDP)](ClO4)2.2(CH2Cl2) _chemical_formula_sum 'C36 H28 Cl6 N6 O8 Ru S2' _chemical_formula_weight 1050.53 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' 'S' 'S' 0.1246 0.1234 '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.759(17) _cell_length_b 17.05(2) _cell_length_c 19.59(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.377(10) _cell_angle_gamma 90.00 _cell_volume 4250(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 0.902 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.466 _exptl_absorpt_correction_T_max 1.000 _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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6871 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.93 _reflns_number_total 6871 _reflns_number_gt 3989 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.1687P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6871 _refine_ls_number_parameters 543 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1466 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2547 _refine_ls_wR_factor_gt 0.2244 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.051 _refine_ls_shift/su_mean 0.006 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.80626(4) 0.02186(4) 0.77908(3) 0.0583(3) Uani 1 d . . . S18 S 0.72558(16) -0.09576(12) 0.74758(11) 0.0672(6) Uani 1 d . . . C181 C 0.6571(6) -0.1348(4) 0.8181(4) 0.0617(18) Uani 1 d . . . N182 N 0.7242(5) -0.1756(4) 0.8584(4) 0.084(2) Uani 1 d . . . C183 C 0.6813(10) -0.2094(7) 0.9113(6) 0.114(4) Uani 1 d . . . H183 H 0.7253 -0.2387 0.9416 0.137 Uiso 1 calc R . . C184 C 0.5819(12) -0.2042(7) 0.9236(6) 0.112(4) Uani 1 d . . . H184 H 0.5566 -0.2328 0.9593 0.135 Uiso 1 calc R . . C185 C 0.5170(8) -0.1582(7) 0.8854(6) 0.101(3) Uani 1 d . . . H185 H 0.4483 -0.1500 0.8965 0.121 Uiso 1 calc R . . C186 C 0.5540(6) -0.1236(5) 0.8296(4) 0.076(2) Uani 1 d . . . H186 H 0.5104 -0.0931 0.8001 0.091 Uiso 1 calc R . . N11 N 0.6873(5) 0.0792(4) 0.7178(3) 0.0706(18) Uani 1 d . . . C12 C 0.6797(6) 0.1602(6) 0.7161(5) 0.091(3) Uani 1 d . . . H12 H 0.7336 0.1892 0.7386 0.110 Uiso 1 calc R . . C13 C 0.5992(7) 0.1994(6) 0.6840(6) 0.106(3) Uani 1 d . . . H13 H 0.5996 0.2539 0.6829 0.127 Uiso 1 calc R . . C14 C 0.5143(8) 0.1578(7) 0.6519(6) 0.107(3) Uani 1 d . . . H14 H 0.4569 0.1842 0.6307 0.129 Uiso 1 calc R . . C15 C 0.5176(6) 0.0775(6) 0.6524(5) 0.089(3) Uani 1 d . . . H15 H 0.4625 0.0485 0.6313 0.106 Uiso 1 calc R . . C16 C 0.6044(7) 0.0397(5) 0.6847(4) 0.073(2) Uani 1 d . . . S17 S 0.6091(2) -0.06188(15) 0.67457(13) 0.0955(8) Uani 1 d . . . N41 N 0.9059(4) 0.0190(4) 0.6981(3) 0.0606(15) Uani 1 d . . . C42 C 0.9757(5) 0.0795(5) 0.7003(4) 0.0634(19) Uani 1 d . . . C43 C 0.9860(7) -0.0282(6) 0.5995(4) 0.085(3) Uani 1 d . . . H43 H 0.9880 -0.0660 0.5654 0.102 Uiso 1 calc R . . C46 C 0.9098(7) -0.0336(5) 0.6486(4) 0.081(2) Uani 1 d . . . H46 H 0.8618 -0.0748 0.6459 0.098 Uiso 1 calc R . . C44 C 1.0547(7) 0.0311(6) 0.6022(5) 0.084(3) Uani 1 d . . . H44 H 1.1039 0.0341 0.5696 0.101 Uiso 1 calc R . . C45 C 1.0542(6) 0.0887(5) 0.6532(4) 0.072(2) Uani 1 d . . . C47 C 0.9705(5) 0.1347(4) 0.7544(4) 0.0606(18) Uani 1 d . . . C48 C 1.0411(6) 0.1982(5) 0.7617(4) 0.073(2) Uani 1 d . . . C49 C 1.0317(7) 0.2516(5) 0.8136(5) 0.086(2) Uani 1 d . . . H49 H 1.0767 0.2945 0.8189 0.103 Uiso 1 calc R . . C50 C 0.9518(7) 0.2395(5) 0.8588(4) 0.079(2) Uani 1 d . . . H50 H 0.9430 0.2747 0.8941 0.095 Uiso 1 calc R . . C51 C 0.8879(6) 0.1759(5) 0.8501(4) 0.073(2) Uani 1 d . . . H51 H 0.8374 0.1679 0.8812 0.088 Uiso 1 calc R . . N52 N 0.8937(4) 0.1247(3) 0.7997(3) 0.0598(15) Uani 1 d . . . C53 C 1.1235(7) 0.1530(6) 0.6610(5) 0.090(3) Uani 1 d . . . H53 H 1.1739 0.1590 0.6296 0.108 Uiso 1 calc R . . C54 C 1.1203(6) 0.2057(6) 0.7113(5) 0.086(3) Uani 1 d . . . H54 H 1.1680 0.2470 0.7144 0.103 Uiso 1 calc R . . N21 N 0.9109(5) -0.0377(3) 0.8478(3) 0.0607(15) Uani 1 d . . . C22 C 1.0008(5) -0.0722(5) 0.8364(4) 0.0646(19) Uani 1 d . . . H22 H 1.0265 -0.0672 0.7935 0.078 Uiso 1 calc R . . C23 C 1.0581(6) -0.1154(5) 0.8864(5) 0.084(2) Uani 1 d . . . H23 H 1.1200 -0.1403 0.8765 0.101 Uiso 1 calc R . . C24 C 1.0222(8) -0.1212(6) 0.9514(5) 0.097(3) Uani 1 d . . . H24 H 1.0603 -0.1503 0.9848 0.116 Uiso 1 calc R . . C25 C 0.9313(6) -0.0845(5) 0.9668(4) 0.069(2) Uani 1 d . . . C26 C 0.8786(6) -0.0429(4) 0.9126(4) 0.0641(19) Uani 1 d . . . C27 C 0.7804(6) -0.0052(5) 0.9240(4) 0.066(2) Uani 1 d . . . C28 C 0.7415(8) -0.0077(6) 0.9909(4) 0.085(3) Uani 1 d . . . C29 C 0.6473(9) 0.0307(6) 0.9989(6) 0.094(3) Uani 1 d . . . H29 H 0.6196 0.0315 1.0415 0.112 Uiso 1 calc R . . C30 C 0.5941(8) 0.0682(6) 0.9431(6) 0.093(3) Uani 1 d . . . H30 H 0.5315 0.0947 0.9484 0.111 Uiso 1 calc R . . C34 C 0.8922(8) -0.0875(6) 1.0322(5) 0.090(3) Uani 1 d . . . H34 H 0.9285 -0.1156 1.0672 0.108 Uiso 1 calc R . . C31 C 0.6369(6) 0.0652(5) 0.8777(5) 0.080(2) Uani 1 d . . . H31 H 0.5993 0.0883 0.8404 0.096 Uiso 1 calc R . . N32 N 0.7277(5) 0.0311(4) 0.8683(3) 0.0667(17) Uani 1 d . . . C33 C 0.8040(9) -0.0503(6) 1.0441(5) 0.095(3) Uani 1 d . . . H33 H 0.7812 -0.0515 1.0880 0.114 Uiso 1 calc R . . Cl1 Cl 0.2877(2) -0.0271(3) 0.76446(17) 0.1339(14) Uani 1 d . . . O11 O 0.3181(10) -0.0335(10) 0.7034(5) 0.274(9) Uani 1 d . . . O12 O 0.1974(7) 0.0119(8) 0.7736(6) 0.208(6) Uani 1 d . . . O13 O 0.2939(9) -0.0930(9) 0.8057(9) 0.252(8) Uani 1 d . . . O14 O 0.3759(10) 0.0181(9) 0.8014(8) 0.225(6) Uani 1 d . . . Cl2 Cl 0.7780(3) -0.20672(19) 0.52107(17) 0.1222(11) Uani 1 d . . . O21 O 0.7449(17) -0.1368(9) 0.5021(8) 0.316(11) Uani 1 d . . . O22 O 0.7374(15) -0.2659(10) 0.4978(7) 0.280(9) Uani 1 d . . . O23 O 0.8836(9) -0.2041(10) 0.5026(6) 0.228(7) Uani 1 d . . . O24 O 0.7805(9) -0.2080(7) 0.5938(5) 0.206(6) Uani 1 d . . . C91 C 0.6908(16) 0.0544(13) 0.4666(11) 0.110(6) Uiso 0.60 d P . . C92 C 0.678(3) 0.014(2) 0.4933(18) 0.129(11) Uiso 0.40 d P . . Cl92 Cl 0.5698(3) 0.1031(4) 0.4736(2) 0.198(2) Uani 1 d . . . Cl93 Cl 0.7920(13) 0.0848(9) 0.5249(8) 0.151(6) Uani 0.50 d P . . Cl94 Cl 0.796(3) 0.100(2) 0.5016(14) 0.173(12) Uiso 0.25 d P . . Cl95 Cl 0.762(2) 0.0891(16) 0.5402(14) 0.134(8) Uiso 0.25 d P . . Cl82 Cl 0.4906(6) 0.2589(5) 0.8363(6) 0.277(5) Uani 0.75 d PD . . Cl83 Cl 0.3020(5) 0.2244(5) 0.8866(3) 0.281(4) Uani 1 d D . . Cl84 Cl 0.3771(13) 0.3096(10) 0.7929(8) 0.152(5) Uiso 0.25 d PD . . C82 C 0.395(3) 0.173(2) 0.8314(19) 0.186(14) Uiso 0.50 d PD . . C83 C 0.380(3) 0.221(2) 0.8140(18) 0.178(13) Uiso 0.50 d PD . . 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 0.0576(4) 0.0561(5) 0.0618(5) 0.0010(3) 0.0080(3) 0.0010(3) S18 0.0711(12) 0.0607(12) 0.0690(12) -0.0001(9) 0.0004(10) 0.0014(9) C181 0.064(4) 0.051(4) 0.069(5) -0.001(4) -0.006(4) -0.004(3) N182 0.085(5) 0.072(5) 0.096(5) 0.027(4) 0.009(4) -0.002(4) C183 0.112(9) 0.111(9) 0.115(9) 0.026(7) -0.017(7) -0.002(7) C184 0.147(11) 0.086(8) 0.109(9) 0.004(6) 0.035(8) -0.026(7) C185 0.086(6) 0.103(8) 0.115(9) -0.022(7) 0.015(6) -0.003(6) C186 0.074(5) 0.081(6) 0.071(5) -0.009(4) 0.000(4) -0.006(4) N11 0.064(4) 0.072(5) 0.074(4) 0.011(3) 0.001(3) -0.010(3) C12 0.073(5) 0.062(6) 0.136(9) 0.015(5) -0.010(6) 0.000(4) C13 0.078(6) 0.075(7) 0.162(10) 0.019(6) -0.012(6) 0.004(5) C14 0.090(7) 0.094(8) 0.134(9) 0.024(7) -0.013(6) 0.016(6) C15 0.069(5) 0.088(7) 0.103(7) 0.017(6) -0.025(5) -0.007(5) C16 0.076(5) 0.062(5) 0.081(6) 0.027(4) 0.006(4) 0.005(4) S17 0.1198(19) 0.0738(16) 0.0862(16) 0.0006(13) -0.0354(14) -0.0120(14) N41 0.056(3) 0.071(4) 0.055(4) 0.005(3) 0.006(3) 0.005(3) C42 0.041(4) 0.079(5) 0.069(5) 0.013(4) -0.007(3) 0.002(4) C43 0.090(6) 0.110(8) 0.056(5) -0.015(5) 0.013(4) 0.004(5) C46 0.080(6) 0.097(7) 0.068(5) 0.000(5) 0.012(4) 0.002(5) C44 0.067(5) 0.115(8) 0.072(6) 0.013(5) 0.015(4) 0.003(5) C45 0.060(4) 0.100(7) 0.056(5) 0.016(4) 0.009(4) 0.013(4) C47 0.052(4) 0.065(5) 0.064(5) 0.012(4) -0.002(3) -0.001(3) C48 0.064(5) 0.068(5) 0.085(6) 0.015(5) 0.002(4) 0.003(4) C49 0.091(6) 0.066(6) 0.097(7) 0.007(5) -0.016(5) -0.015(5) C50 0.092(6) 0.060(5) 0.084(6) -0.002(4) 0.000(5) -0.007(4) C51 0.091(5) 0.065(5) 0.064(5) -0.011(4) 0.001(4) -0.003(4) N52 0.053(3) 0.061(4) 0.064(4) 0.008(3) -0.005(3) -0.004(3) C53 0.072(5) 0.109(8) 0.089(7) 0.018(6) 0.014(5) -0.008(5) C54 0.065(5) 0.095(7) 0.098(7) 0.026(6) 0.005(5) -0.013(4) N21 0.065(4) 0.057(4) 0.061(4) -0.001(3) 0.014(3) 0.000(3) C22 0.056(4) 0.071(5) 0.067(5) 0.003(4) 0.004(4) 0.003(4) C23 0.068(5) 0.071(6) 0.112(8) 0.004(5) 0.000(5) 0.001(4) C24 0.125(8) 0.081(6) 0.079(6) 0.016(5) -0.026(6) -0.010(6) C25 0.065(5) 0.076(5) 0.065(5) 0.006(4) -0.003(4) -0.005(4) C26 0.070(5) 0.061(5) 0.061(5) 0.001(4) 0.004(4) -0.015(4) C27 0.080(5) 0.060(5) 0.059(5) -0.006(4) 0.012(4) -0.017(4) C28 0.112(7) 0.074(6) 0.071(6) -0.014(5) 0.031(5) -0.038(5) C29 0.105(7) 0.085(7) 0.097(7) -0.017(6) 0.049(6) -0.022(6) C30 0.084(6) 0.089(7) 0.110(8) -0.019(6) 0.036(6) -0.007(5) C34 0.092(6) 0.109(8) 0.068(6) 0.007(5) -0.003(5) -0.013(6) C31 0.064(5) 0.078(6) 0.100(7) -0.002(5) 0.022(5) 0.012(4) N32 0.062(4) 0.065(4) 0.076(4) -0.004(3) 0.019(3) -0.006(3) C33 0.126(8) 0.103(7) 0.054(5) 0.018(5) 0.000(5) -0.026(6) Cl1 0.0871(19) 0.210(4) 0.106(2) 0.035(2) 0.0219(17) 0.050(2) O11 0.205(11) 0.51(3) 0.120(8) -0.072(11) 0.089(8) -0.117(14) O12 0.107(6) 0.303(14) 0.220(12) 0.138(11) 0.039(7) 0.077(7) O13 0.180(11) 0.248(16) 0.337(18) 0.148(15) 0.067(11) 0.069(10) O14 0.151(10) 0.249(16) 0.268(16) -0.044(12) -0.035(10) 0.053(9) Cl2 0.162(3) 0.089(2) 0.124(2) -0.0146(17) 0.065(2) -0.0309(19) O21 0.53(3) 0.141(12) 0.284(19) 0.019(11) 0.11(2) 0.118(15) O22 0.40(2) 0.192(15) 0.239(15) -0.062(11) -0.027(15) -0.113(14) O23 0.154(8) 0.36(2) 0.171(9) 0.024(10) 0.052(8) -0.042(11) O24 0.226(10) 0.261(14) 0.142(8) -0.044(8) 0.098(8) -0.128(10) Cl92 0.172(3) 0.295(6) 0.123(3) 0.011(3) -0.025(3) 0.079(4) Cl93 0.180(11) 0.151(9) 0.109(8) -0.038(7) -0.061(7) 0.082(8) Cl82 0.191(6) 0.187(7) 0.456(15) -0.071(9) 0.047(8) 0.008(6) Cl83 0.242(6) 0.414(11) 0.187(5) 0.045(6) 0.019(4) -0.110(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 N32 2.086(6) . ? Ru1 N21 2.087(6) . ? Ru1 N52 2.101(6) . ? Ru1 N11 2.103(7) . ? Ru1 N41 2.108(6) . ? Ru1 S18 2.316(3) . ? S18 C181 1.818(7) . ? S18 S17 2.065(4) . ? C181 N182 1.316(10) . ? C181 C186 1.365(10) . ? N182 C183 1.340(13) . ? C183 C184 1.313(15) . ? C184 C185 1.329(15) . ? C185 C186 1.358(13) . ? N11 C16 1.374(10) . ? N11 C12 1.385(11) . ? C12 C13 1.342(12) . ? C13 C14 1.403(14) . ? C14 C15 1.370(13) . ? C15 C16 1.392(12) . ? C16 S17 1.744(9) . ? N41 C46 1.325(10) . ? N41 C42 1.361(10) . ? C42 C45 1.422(10) . ? C42 C47 1.423(11) . ? C43 C44 1.336(12) . ? C43 C46 1.422(11) . ? C44 C45 1.402(12) . ? C45 C53 1.409(13) . ? C47 N52 1.381(8) . ? C47 C48 1.409(10) . ? C48 C49 1.377(12) . ? C48 C54 1.472(11) . ? C49 C50 1.416(11) . ? C50 C51 1.359(11) . ? C51 N52 1.325(9) . ? C53 C54 1.336(13) . ? N21 C22 1.322(8) . ? N21 C26 1.367(9) . ? C22 C23 1.389(11) . ? C23 C24 1.388(12) . ? C24 C25 1.372(12) . ? C25 C26 1.405(11) . ? C25 C34 1.410(11) . ? C26 C27 1.441(11) . ? C27 N32 1.384(10) . ? C27 C28 1.438(10) . ? C28 C29 1.388(14) . ? C28 C33 1.456(14) . ? C29 C30 1.398(14) . ? C30 C31 1.431(12) . ? C34 C33 1.328(13) . ? C31 N32 1.322(9) . ? Cl1 O11 1.291(9) . ? Cl1 O12 1.354(10) . ? Cl1 O13 1.382(12) . ? Cl1 O14 1.503(14) . ? Cl2 O22 1.208(13) . ? Cl2 O21 1.310(14) . ? Cl2 O23 1.422(10) . ? Cl2 O24 1.422(10) . ? C91 C92 0.89(3) . ? C91 Cl94 1.66(4) . ? C91 Cl93 1.74(3) . ? C91 Cl95 1.75(3) . ? C91 Cl92 1.77(2) . ? C92 Cl95 1.87(5) . ? C92 Cl93 1.96(4) . ? C92 Cl92 2.07(4) . ? C92 Cl94 2.10(5) . ? Cl93 Cl95 0.51(3) . ? Cl93 Cl94 0.54(4) . ? Cl94 Cl95 0.92(4) . ? Cl82 C83 1.58(4) . ? Cl82 Cl84 1.839(19) . ? Cl82 C82 1.91(3) . ? Cl83 C83 1.80(3) . ? Cl83 C82 1.88(3) . ? Cl84 C83 1.57(3) . ? C82 C83 0.91(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 N32 Ru1 N21 79.7(2) . . ? N32 Ru1 N52 93.3(2) . . ? N21 Ru1 N52 88.7(2) . . ? N32 Ru1 N11 94.1(3) . . ? N21 Ru1 N11 173.3(2) . . ? N52 Ru1 N11 94.1(3) . . ? N32 Ru1 N41 171.2(2) . . ? N21 Ru1 N41 94.7(2) . . ? N52 Ru1 N41 79.7(2) . . ? N11 Ru1 N41 91.8(2) . . ? N32 Ru1 S18 93.22(18) . . ? N21 Ru1 S18 90.00(19) . . ? N52 Ru1 S18 172.98(16) . . ? N11 Ru1 S18 87.9(2) . . ? N41 Ru1 S18 93.49(19) . . ? C181 S18 S17 105.5(3) . . ? C181 S18 Ru1 110.2(2) . . ? S17 S18 Ru1 102.95(13) . . ? N182 C181 C186 124.5(7) . . ? N182 C181 S18 108.7(5) . . ? C186 C181 S18 126.8(6) . . ? C181 N182 C183 113.9(8) . . ? C184 C183 N182 124.8(11) . . ? C183 C184 C185 120.4(11) . . ? C184 C185 C186 118.0(9) . . ? C185 C186 C181 118.1(9) . . ? C16 N11 C12 115.4(7) . . ? C16 N11 Ru1 122.5(5) . . ? C12 N11 Ru1 121.5(6) . . ? C13 C12 N11 123.8(9) . . ? C12 C13 C14 119.7(9) . . ? C15 C14 C13 118.7(9) . . ? C14 C15 C16 119.3(9) . . ? N11 C16 C15 123.0(8) . . ? N11 C16 S17 120.6(6) . . ? C15 C16 S17 116.2(7) . . ? C16 S17 S18 103.2(3) . . ? C46 N41 C42 118.4(6) . . ? C46 N41 Ru1 128.7(6) . . ? C42 N41 Ru1 112.9(5) . . ? N41 C42 C45 123.7(8) . . ? N41 C42 C47 117.2(6) . . ? C45 C42 C47 119.1(7) . . ? C44 C43 C46 120.2(8) . . ? N41 C46 C43 121.2(8) . . ? C43 C44 C45 121.3(8) . . ? C44 C45 C53 125.9(7) . . ? C44 C45 C42 115.3(8) . . ? C53 C45 C42 118.8(8) . . ? N52 C47 C48 120.6(7) . . ? N52 C47 C42 118.2(6) . . ? C48 C47 C42 121.2(6) . . ? C49 C48 C47 119.5(7) . . ? C49 C48 C54 122.8(8) . . ? C47 C48 C54 117.7(8) . . ? C48 C49 C50 118.2(8) . . ? C51 C50 C49 119.5(8) . . ? N52 C51 C50 123.4(7) . . ? C51 N52 C47 118.7(6) . . ? C51 N52 Ru1 129.3(5) . . ? C47 N52 Ru1 111.8(5) . . ? C54 C53 C45 123.3(8) . . ? C53 C54 C48 119.8(8) . . ? C22 N21 C26 117.1(7) . . ? C22 N21 Ru1 128.8(5) . . ? C26 N21 Ru1 114.0(5) . . ? N21 C22 C23 122.2(7) . . ? C24 C23 C22 119.5(8) . . ? C25 C24 C23 120.9(8) . . ? C24 C25 C26 115.2(7) . . ? C24 C25 C34 123.2(9) . . ? C26 C25 C34 121.6(8) . . ? N21 C26 C25 125.0(7) . . ? N21 C26 C27 116.3(7) . . ? C25 C26 C27 118.6(7) . . ? N32 C27 C28 123.5(8) . . ? N32 C27 C26 117.0(6) . . ? C28 C27 C26 119.5(8) . . ? C29 C28 C27 116.8(10) . . ? C29 C28 C33 125.9(9) . . ? C27 C28 C33 117.3(9) . . ? C28 C29 C30 120.0(8) . . ? C29 C30 C31 119.3(8) . . ? C33 C34 C25 120.3(9) . . ? N32 C31 C30 122.6(9) . . ? C31 N32 C27 117.7(7) . . ? C31 N32 Ru1 129.3(6) . . ? C27 N32 Ru1 113.0(5) . . ? C34 C33 C28 122.6(8) . . ? O11 Cl1 O12 118.9(9) . . ? O11 Cl1 O13 117.8(11) . . ? O12 Cl1 O13 109.5(7) . . ? O11 Cl1 O14 102.9(9) . . ? O12 Cl1 O14 107.4(9) . . ? O13 Cl1 O14 97.3(10) . . ? O22 Cl2 O21 122.2(14) . . ? O22 Cl2 O23 108.5(11) . . ? O21 Cl2 O23 101.0(10) . . ? O22 Cl2 O24 110.0(8) . . ? O21 Cl2 O24 106.2(9) . . ? O23 Cl2 O24 107.8(8) . . ? C92 C91 Cl94 108(3) . . ? C92 C91 Cl93 90(3) . . ? Cl94 C91 Cl93 17.9(14) . . ? C92 C91 Cl95 83(3) . . ? Cl94 C91 Cl95 31.1(13) . . ? Cl93 C91 Cl95 16.7(11) . . ? C92 C91 Cl92 97(3) . . ? Cl94 C91 Cl92 115.4(18) . . ? Cl93 C91 Cl92 114.7(12) . . ? Cl95 C91 Cl92 100.4(13) . . ? C91 C92 Cl95 68(3) . . ? C91 C92 Cl93 63(3) . . ? Cl95 C92 Cl93 14.9(10) . . ? C91 C92 Cl92 58(3) . . ? Cl95 C92 Cl92 86.5(17) . . ? Cl93 C92 Cl92 94.2(16) . . ? C91 C92 Cl94 49(3) . . ? Cl95 C92 Cl94 25.8(13) . . ? Cl93 C92 Cl94 14.6(10) . . ? Cl92 C92 Cl94 87.8(17) . . ? C91 Cl92 C92 25.3(10) . . ? Cl95 Cl93 Cl94 124(7) . . ? Cl95 Cl93 C91 83(4) . . ? Cl94 Cl93 C91 72(4) . . ? Cl95 Cl93 C92 73(5) . . ? Cl94 Cl93 C92 99(5) . . ? C91 Cl93 C92 27.0(11) . . ? Cl93 Cl94 Cl95 27(4) . . ? Cl93 Cl94 C91 90(5) . . ? Cl95 Cl94 C91 80(3) . . ? Cl93 Cl94 C92 67(5) . . ? Cl95 Cl94 C92 63(3) . . ? C91 Cl94 C92 23.7(12) . . ? Cl93 Cl95 Cl94 29(4) . . ? Cl93 Cl95 C91 80(4) . . ? Cl94 Cl95 C91 69(3) . . ? Cl93 Cl95 C92 92(5) . . ? Cl94 Cl95 C92 91(3) . . ? C91 Cl95 C92 28.2(12) . . ? C83 Cl82 Cl84 53.9(13) . . ? C83 Cl82 C82 28.1(16) . . ? Cl84 Cl82 C82 82.0(14) . . ? C83 Cl83 C82 28.3(14) . . ? C83 Cl84 Cl82 54.6(16) . . ? C83 C82 Cl83 71(3) . . ? C83 C82 Cl82 55(3) . . ? Cl83 C82 Cl82 92.2(15) . . ? C82 C83 Cl84 168(5) . . ? C82 C83 Cl82 96(4) . . ? Cl84 C83 Cl82 71.5(18) . . ? C82 C83 Cl83 81(3) . . ? Cl84 C83 Cl83 100.0(19) . . ? Cl82 C83 Cl83 108(2) . . ? _refine_diff_density_max 0.919 _refine_diff_density_min -1.005 _refine_diff_density_rms 0.107