# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'P. Raithby' _publ_contact_author_address ; Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UNITED KINGDOM ; _publ_contact_author_email P.R.RAITHBY@BATH.AC.UK _publ_section_title ; Photocrystallographic Structure Determination of a New Geometric Isomer of [Ru(NH3)4(H2O)(?1-OSO)][MeC6H4SO3]2 ; loop_ _publ_author_name 'P Raithby' 'Katharine F. Bowes' 'Jacqueline M. Cole' 'Shamus L. G. Husheer' 'Teresa L. Savarese' ; H.A.Sparkes ; 'Simon J. Teat' 'John E. Warren' data_e:\datasets\rut72\rut72 _database_code_depnum_ccdc_archive 'CCDC 602437' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H28 N4 O9 Ru S3' _chemical_formula_weight 593.65 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' S S 0.1246 0.1234 '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 6.655(3) _cell_length_b 13.109(6) _cell_length_c 13.715(6) _cell_angle_alpha 91.663(4) _cell_angle_beta 96.450(4) _cell_angle_gamma 104.721(4) _cell_volume 1147.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 13(2) _cell_measurement_reflns_used 3303 _cell_measurement_theta_min 2.914 _cell_measurement_theta_max 29.638 _exptl_crystal_description plate _exptl_crystal_colour 'pale orange' _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 1.008 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8288 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS, (G. Sheldrick, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 13(2) _diffrn_radiation_wavelength 0.68960 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13556 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0745 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 30.91 _reflns_number_total 7121 _reflns_number_gt 5282 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^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 7121 _refine_ls_number_parameters 400 _refine_ls_number_restraints 395 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0976 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.004 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 0.32525(4) 0.99214(2) 0.252870(18) 0.01676(7) Uani 1 1 d D . . S1 S 0.3934(3) 0.84872(13) 0.21594(13) 0.0187(3) Uani 0.56 1 d PU A 1 O1 O 0.2914(7) 0.7508(3) 0.2558(3) 0.0231(7) Uani 0.56 1 d PU A 1 O2 O 0.5377(7) 0.8414(3) 0.1454(3) 0.0209(8) Uani 0.56 1 d PU A 1 N1 N 0.6354(4) 1.0711(2) 0.3150(2) 0.0220(6) Uani 1 1 d . A . H1A H 0.6985 1.0236 0.3436 0.033 Uiso 1 1 calc R . . H1B H 0.6310 1.1215 0.3612 0.033 Uiso 1 1 calc R . . H1C H 0.7093 1.1020 0.2669 0.033 Uiso 1 1 calc R . . N2 N 0.2659(4) 0.9504(2) 0.39692(19) 0.0207(5) Uani 1 1 d . A . H2A H 0.1253 0.9308 0.3993 0.031 Uiso 1 1 calc R . . H2B H 0.3256 1.0069 0.4401 0.031 Uiso 1 1 calc R . . H2C H 0.3214 0.8956 0.4133 0.031 Uiso 1 1 calc R . . N3 N 0.0053(4) 0.9330(2) 0.19899(19) 0.0199(5) Uani 1 1 d . A . H3A H -0.0084 0.8862 0.1468 0.030 Uiso 1 1 calc R . . H3B H -0.0488 0.9874 0.1796 0.030 Uiso 1 1 calc R . . H3C H -0.0650 0.8999 0.2473 0.030 Uiso 1 1 calc R . . N4 N 0.3810(4) 1.0410(2) 0.10970(19) 0.0215(5) Uani 1 1 d . A . H4A H 0.5213 1.0603 0.1064 0.032 Uiso 1 1 calc R . . H4B H 0.3268 1.0971 0.0969 0.032 Uiso 1 1 calc R . . H4C H 0.3187 0.9867 0.0646 0.032 Uiso 1 1 calc R . . O1W O 0.2633(4) 1.13712(18) 0.28357(16) 0.0215(5) Uani 1 1 d D A . H1W H 0.201(5) 1.142(3) 0.3330(19) 0.032 Uiso 1 1 d D . . H2W H 0.241(6) 1.170(3) 0.2339(18) 0.032 Uiso 1 1 d D . . S11 S -0.03332(11) 1.20537(6) 0.07716(6) 0.01779(15) Uani 1 1 d . . . O11 O -0.0858(4) 1.1712(2) -0.02548(18) 0.0334(6) Uani 1 1 d . . . O12 O 0.1904(3) 1.22495(18) 0.11158(19) 0.0264(5) Uani 1 1 d . . . O13 O -0.1568(4) 1.13145(18) 0.13922(19) 0.0280(5) Uani 1 1 d . . . C11 C -0.0962(5) 1.3273(2) 0.0933(2) 0.0165(6) Uani 1 1 d . . . C12 C -0.2990(5) 1.3333(2) 0.0652(2) 0.0215(6) Uani 1 1 d . . . H12 H -0.4016 1.2733 0.0348 0.026 Uiso 1 1 calc R . . C13 C -0.3512(5) 1.4278(2) 0.0818(2) 0.0205(6) Uani 1 1 d . . . H13 H -0.4913 1.4313 0.0637 0.025 Uiso 1 1 calc R . . C14 C -0.2026(5) 1.5177(2) 0.1244(2) 0.0201(6) Uani 1 1 d . . . C15 C 0.0029(5) 1.5105(2) 0.1501(2) 0.0229(7) Uani 1 1 d . . . H15 H 0.1070 1.5712 0.1780 0.028 Uiso 1 1 calc R . . C16 C 0.0567(5) 1.4163(2) 0.1354(2) 0.0206(6) Uani 1 1 d . . . H16 H 0.1963 1.4123 0.1537 0.025 Uiso 1 1 calc R . . C17 C -0.2607(6) 1.6200(3) 0.1423(3) 0.0262(7) Uani 1 1 d . . . H17A H -0.1870 1.6545 0.2053 0.039 Uiso 1 1 calc R . . H17B H -0.4121 1.6054 0.1439 0.039 Uiso 1 1 calc R . . H17C H -0.2206 1.6667 0.0892 0.039 Uiso 1 1 calc R . . S21 S -0.26426(12) 0.81673(6) 0.46622(6) 0.01775(15) Uani 1 1 d . . . O21 O -0.2055(4) 0.87935(18) 0.38208(18) 0.0275(5) Uani 1 1 d . . . O22 O -0.0991(3) 0.84465(17) 0.54968(17) 0.0232(5) Uani 1 1 d . . . O23 O -0.4673(3) 0.82337(17) 0.49289(16) 0.0204(5) Uani 1 1 d . . . C21 C -0.2851(5) 0.6838(2) 0.4299(2) 0.0170(6) Uani 1 1 d . . . C22 C -0.1030(5) 0.6500(2) 0.4289(2) 0.0206(6) Uani 1 1 d . . . H22 H 0.0297 0.6976 0.4495 0.025 Uiso 1 1 calc R . . C23 C -0.1160(5) 0.5472(2) 0.3979(2) 0.0234(7) Uani 1 1 d . . . H23 H 0.0088 0.5249 0.3966 0.028 Uiso 1 1 calc R . . C24 C -0.3079(6) 0.4758(2) 0.3685(2) 0.0257(7) Uani 1 1 d . . . C25 C -0.4888(5) 0.5106(3) 0.3701(2) 0.0267(8) Uani 1 1 d . . . H25 H -0.6213 0.4624 0.3506 0.032 Uiso 1 1 calc R . . C26 C -0.4795(5) 0.6139(3) 0.3996(2) 0.0235(7) Uani 1 1 d . . . H26 H -0.6041 0.6368 0.3991 0.028 Uiso 1 1 calc R . . C27 C -0.3190(6) 0.3625(2) 0.3389(3) 0.0330(9) Uani 1 1 d . . . H27A H -0.1795 0.3565 0.3278 0.050 Uiso 1 1 calc R . . H27B H -0.4157 0.3404 0.2782 0.050 Uiso 1 1 calc R . . H27C H -0.3692 0.3171 0.3913 0.050 Uiso 1 1 calc R . . S1A S 0.4569(5) 0.7935(3) 0.1753(3) 0.0200(5) Uani 0.24 1 d PDU A 2 S1B S 0.3790(11) 0.7709(5) 0.2243(5) 0.0205(7) Uani 0.12 1 d PDU A 3 O2A O 0.554(2) 0.8547(12) 0.1010(11) 0.0190(16) Uani 0.24 1 d PDU A 2 S1C S 0.502(2) 0.8534(11) 0.2131(11) 0.0196(8) Uani 0.06 1 d PDU A 4 O1A O 0.3504(19) 0.8494(9) 0.2437(8) 0.0204(8) Uani 0.24 1 d PDU A 2 O1B O 0.222(3) 0.7398(17) 0.2881(14) 0.0204(17) Uani 0.12 1 d PDU A 3 O1C O 0.273(6) 0.8130(8) 0.220(3) 0.0196(8) Uani 0.06 1 d PDU A 4 O2D O 0.336(17) 0.833(5) 0.172(3) 0.0199(8) Uani 0.02 1 d PDU A 5 O2B O 0.456(3) 0.8875(9) 0.2076(15) 0.0203(8) Uani 0.12 1 d PDU A 3 S1D S 0.437(5) 0.8276(18) 0.281(3) 0.0201(8) Uani 0.02 1 d PDU A 5 O1D O 0.272(16) 0.733(7) 0.316(8) 0.021(2) Uani 0.02 1 d PDU A 5 O2C O 0.589(9) 0.866(5) 0.111(4) 0.020(2) Uani 0.06 1 d PDU A 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01436(11) 0.01960(12) 0.01613(12) 0.00017(8) 0.00223(8) 0.00399(8) S1 0.0171(8) 0.0182(6) 0.0219(8) 0.0026(6) 0.0041(6) 0.0055(5) O1 0.0221(17) 0.0204(15) 0.0262(17) -0.0004(14) 0.0039(14) 0.0042(14) O2 0.0188(17) 0.0207(17) 0.0234(18) 0.0016(16) 0.0042(16) 0.0047(14) N1 0.0192(13) 0.0226(13) 0.0231(14) -0.0007(11) 0.0013(11) 0.0044(10) N2 0.0226(13) 0.0193(13) 0.0199(13) -0.0001(10) 0.0034(10) 0.0047(10) N3 0.0195(12) 0.0194(13) 0.0203(13) 0.0004(10) 0.0022(10) 0.0045(10) N4 0.0175(12) 0.0282(14) 0.0196(13) 0.0013(11) 0.0039(10) 0.0067(10) O1W 0.0233(11) 0.0253(12) 0.0174(11) 0.0015(9) 0.0022(9) 0.0089(9) S11 0.0157(3) 0.0176(3) 0.0210(4) 0.0013(3) 0.0047(3) 0.0048(3) O11 0.0455(16) 0.0324(14) 0.0248(13) -0.0076(10) -0.0010(11) 0.0180(12) O12 0.0163(10) 0.0228(11) 0.0409(14) 0.0048(10) 0.0059(10) 0.0053(9) O13 0.0244(12) 0.0234(12) 0.0409(15) 0.0107(10) 0.0140(11) 0.0095(9) C11 0.0170(13) 0.0179(14) 0.0144(14) 0.0004(11) 0.0048(11) 0.0028(11) C12 0.0160(14) 0.0211(15) 0.0263(17) 0.0022(12) 0.0034(12) 0.0023(12) C13 0.0162(14) 0.0225(15) 0.0237(16) 0.0033(12) 0.0027(12) 0.0065(11) C14 0.0260(16) 0.0207(15) 0.0157(14) 0.0032(11) 0.0053(12) 0.0084(12) C15 0.0258(16) 0.0186(15) 0.0215(16) -0.0025(12) 0.0041(13) 0.0005(12) C16 0.0194(14) 0.0219(15) 0.0205(15) -0.0008(12) 0.0037(12) 0.0049(12) C17 0.0331(18) 0.0207(15) 0.0269(17) 0.0037(13) 0.0047(14) 0.0100(13) S21 0.0187(3) 0.0141(3) 0.0211(4) 0.0016(3) 0.0083(3) 0.0030(3) O21 0.0395(14) 0.0194(11) 0.0285(13) 0.0088(9) 0.0202(11) 0.0092(10) O22 0.0153(10) 0.0229(11) 0.0292(12) -0.0062(9) 0.0044(9) 0.0014(8) O23 0.0180(10) 0.0251(11) 0.0212(11) 0.0013(9) 0.0083(9) 0.0086(9) C21 0.0196(14) 0.0157(13) 0.0147(14) 0.0022(11) 0.0039(11) 0.0017(11) C22 0.0205(15) 0.0183(14) 0.0221(16) 0.0025(12) 0.0027(12) 0.0035(12) C23 0.0280(16) 0.0207(15) 0.0243(16) 0.0015(12) 0.0079(13) 0.0090(13) C24 0.0388(19) 0.0171(14) 0.0213(16) 0.0016(12) 0.0145(14) 0.0027(13) C25 0.0261(17) 0.0209(15) 0.0269(17) -0.0055(13) 0.0094(14) -0.0068(13) C26 0.0177(14) 0.0246(16) 0.0281(17) 0.0007(13) 0.0090(13) 0.0031(12) C27 0.051(2) 0.0154(15) 0.0333(19) -0.0023(13) 0.0206(17) 0.0028(15) S1A 0.0203(11) 0.0202(10) 0.0193(11) 0.0002(9) 0.0039(9) 0.0043(9) S1B 0.0200(13) 0.0198(12) 0.0212(13) 0.0014(12) 0.0040(12) 0.0035(12) O2A 0.020(3) 0.019(3) 0.019(3) 0.002(3) 0.003(3) 0.007(3) S1C 0.0188(14) 0.0198(13) 0.0210(14) 0.0010(13) 0.0037(13) 0.0058(13) O1A 0.0195(14) 0.0208(13) 0.0214(14) 0.0019(13) 0.0041(13) 0.0054(13) O1B 0.021(3) 0.020(3) 0.022(3) 0.000(3) 0.006(3) 0.006(3) O1C 0.0189(14) 0.0194(13) 0.0209(14) 0.0016(13) 0.0040(13) 0.0048(13) O2D 0.0192(14) 0.0198(13) 0.0211(14) 0.0015(13) 0.0039(13) 0.0049(13) O2B 0.0197(15) 0.0200(14) 0.0212(14) 0.0017(14) 0.0038(13) 0.0046(13) S1D 0.0194(14) 0.0199(13) 0.0212(14) 0.0014(13) 0.0039(13) 0.0050(13) O1D 0.020(3) 0.020(3) 0.022(3) 0.000(3) 0.005(3) 0.005(3) O2C 0.019(3) 0.020(3) 0.020(3) 0.001(3) 0.004(3) 0.006(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 Ru1 O1A 1.923(11) . ? Ru1 O2B 1.923(11) . ? Ru1 O1W 2.086(2) . ? Ru1 S1 2.104(2) . ? Ru1 N3 2.111(3) . ? Ru1 N2 2.118(3) . ? Ru1 N4 2.126(3) . ? Ru1 N1 2.127(3) . ? Ru1 O1C 2.307(8) . ? Ru1 O2D 2.358(19) . ? Ru1 S1D 2.481(15) . ? Ru1 S1C 2.481(14) . ? S1 O1 1.446(5) . ? S1 O2 1.455(5) . ? S11 O11 1.441(3) . ? S11 O13 1.463(2) . ? S11 O12 1.465(2) . ? S11 C11 1.766(3) . ? C11 C12 1.384(4) . ? C11 C16 1.399(4) . ? C12 C13 1.388(4) . ? C13 C14 1.395(4) . ? C14 C15 1.401(5) . ? C14 C17 1.508(4) . ? C15 C16 1.386(4) . ? S21 O23 1.462(2) . ? S21 O22 1.463(2) . ? S21 O21 1.467(2) . ? S21 C21 1.765(3) . ? C21 C26 1.393(4) . ? C21 C22 1.393(4) . ? C22 C23 1.379(4) . ? C23 C24 1.387(5) . ? C24 C25 1.394(5) . ? C24 C27 1.510(4) . ? C25 C26 1.387(5) . ? S1A O2A 1.426(15) . ? S1A O1A 1.514(10) . ? S1B O1B 1.426(15) . ? S1B O2B 1.516(11) . ? S1C O1C 1.49(4) . ? S1C O2C 1.57(6) . ? O2D S1D 1.57(5) . ? S1D O1D 1.57(6) . ? 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 O1A Ru1 O2B 28.6(6) . . ? O1A Ru1 O1W 169.3(3) . . ? O2B Ru1 O1W 161.7(4) . . ? O1A Ru1 S1 13.4(3) . . ? O2B Ru1 S1 16.1(4) . . ? O1W Ru1 S1 177.32(8) . . ? O1A Ru1 N3 87.9(4) . . ? O2B Ru1 N3 104.5(6) . . ? O1W Ru1 N3 87.94(10) . . ? S1 Ru1 N3 92.55(9) . . ? O1A Ru1 N2 81.4(3) . . ? O2B Ru1 N2 104.0(5) . . ? O1W Ru1 N2 88.75(10) . . ? S1 Ru1 N2 93.87(9) . . ? N3 Ru1 N2 91.24(10) . . ? O1A Ru1 N4 101.3(3) . . ? O2B Ru1 N4 78.7(5) . . ? O1W Ru1 N4 88.46(10) . . ? S1 Ru1 N4 88.92(9) . . ? N3 Ru1 N4 88.53(10) . . ? N2 Ru1 N4 177.21(11) . . ? O1A Ru1 N1 99.8(4) . . ? O2B Ru1 N1 83.7(6) . . ? O1W Ru1 N1 83.94(10) . . ? S1 Ru1 N1 95.63(9) . . ? N3 Ru1 N1 171.74(10) . . ? N2 Ru1 N1 87.10(11) . . ? N4 Ru1 N1 92.74(10) . . ? O1A Ru1 O1C 14.3(10) . . ? O2B Ru1 O1C 36.7(9) . . ? O1W Ru1 O1C 160.6(9) . . ? S1 Ru1 O1C 21.0(9) . . ? N3 Ru1 O1C 73.9(9) . . ? N2 Ru1 O1C 84.9(10) . . ? N4 Ru1 O1C 97.7(10) . . ? N1 Ru1 O1C 114.0(9) . . ? O1A Ru1 O2D 24.0(13) . . ? O2B Ru1 O2D 24(3) . . ? O1W Ru1 O2D 162.5(15) . . ? S1 Ru1 O2D 16.0(17) . . ? N3 Ru1 O2D 80(3) . . ? N2 Ru1 O2D 104.3(16) . . ? N4 Ru1 O2D 78.4(15) . . ? N1 Ru1 O2D 108(3) . . ? O1C Ru1 O2D 21(2) . . ? O1A Ru1 S1D 16.4(9) . . ? O2B Ru1 S1D 30.8(10) . . ? O1W Ru1 S1D 159.5(9) . . ? S1 Ru1 S1D 22.6(9) . . ? N3 Ru1 S1D 102.1(9) . . ? N2 Ru1 S1D 73.4(9) . . ? N4 Ru1 S1D 109.4(9) . . ? N1 Ru1 S1D 85.1(9) . . ? O1C Ru1 S1D 30.3(13) . . ? O2D Ru1 S1D 37.8(11) . . ? O1A Ru1 S1C 25.8(4) . . ? O2B Ru1 S1C 6.1(7) . . ? O1W Ru1 S1C 163.3(4) . . ? S1 Ru1 S1C 15.2(3) . . ? N3 Ru1 S1C 106.9(4) . . ? N2 Ru1 S1C 98.3(3) . . ? N4 Ru1 S1C 84.5(3) . . ? N1 Ru1 S1C 81.3(4) . . ? O1C Ru1 S1C 36.1(9) . . ? O2D Ru1 S1C 27(2) . . ? S1D Ru1 S1C 25.4(9) . . ? O1 S1 O2 116.2(3) . . ? O1 S1 Ru1 121.7(2) . . ? O2 S1 Ru1 122.1(2) . . ? O11 S11 O13 111.78(16) . . ? O11 S11 O12 113.34(15) . . ? O13 S11 O12 110.25(15) . . ? O11 S11 C11 107.73(15) . . ? O13 S11 C11 107.08(14) . . ? O12 S11 C11 106.26(14) . . ? C12 C11 C16 120.4(3) . . ? C12 C11 S11 119.3(2) . . ? C16 C11 S11 120.3(2) . . ? C11 C12 C13 119.4(3) . . ? C12 C13 C14 121.5(3) . . ? C13 C14 C15 118.1(3) . . ? C13 C14 C17 121.1(3) . . ? C15 C14 C17 120.8(3) . . ? C16 C15 C14 121.1(3) . . ? C15 C16 C11 119.4(3) . . ? O23 S21 O22 112.31(13) . . ? O23 S21 O21 112.00(14) . . ? O22 S21 O21 111.28(14) . . ? O23 S21 C21 107.88(13) . . ? O22 S21 C21 106.15(14) . . ? O21 S21 C21 106.84(14) . . ? C26 C21 C22 120.0(3) . . ? C26 C21 S21 120.9(2) . . ? C22 C21 S21 119.0(2) . . ? C23 C22 C21 119.8(3) . . ? C22 C23 C24 121.3(3) . . ? C23 C24 C25 118.4(3) . . ? C23 C24 C27 120.4(3) . . ? C25 C24 C27 121.2(3) . . ? C26 C25 C24 121.4(3) . . ? C25 C26 C21 119.1(3) . . ? O2A S1A O1A 116.2(8) . . ? O1B S1B O2B 118.1(11) . . ? O1C S1C O2C 122(3) . . ? O1C S1C Ru1 65.6(7) . . ? O2C S1C Ru1 113(3) . . ? S1A O1A Ru1 132.1(7) . . ? S1C O1C Ru1 78.3(9) . . ? S1D O2D Ru1 75.4(13) . . ? S1B O2B Ru1 123.1(7) . . ? O1D S1D O2D 101(6) . . ? O1D S1D Ru1 116(5) . . ? O2D S1D Ru1 66.9(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 C12 C11 S11 O11 57.1(3) . . . . ? C12 C11 S11 O12 178.9(2) . . . . ? C12 C11 S11 O13 -63.3(3) . . . . ? C22 C21 S21 O21 78.3(3) . . . . ? C22 C21 S21 O22 -40.6(3) . . . . ? C22 C21 S21 O23 -161.1(2) . . . . ? 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 N1 H1A O21 0.91 2.20 3.091(4) 164.6 1_655 N1 H1B O23 0.91 2.55 3.368(4) 149.2 2_576 N1 H1C O13 0.91 2.06 2.942(4) 164.3 1_655 N2 H2A O21 0.91 2.12 3.019(4) 171.4 . N2 H2A S21 0.91 2.91 3.759(3) 156.7 . N2 H2B O22 0.91 2.76 3.251(4) 115.2 2_576 N2 H2B S21 0.91 2.76 3.540(3) 145.1 2_576 N2 H2C O23 0.91 2.11 2.960(4) 154.8 1_655 N3 H3A O11 0.91 2.03 2.879(4) 154.1 2_575 N3 H3A S11 0.91 3.33 4.195(3) 159.2 2_575 N3 H3B O13 0.91 2.25 3.155(4) 174.9 . N3 H3C O21 0.91 2.16 3.027(3) 159.5 . N4 H4A O13 0.91 2.10 2.979(4) 162.1 1_655 N4 H4B S11 0.91 3.07 3.904(3) 152.8 . N4 H4B O12 0.91 2.11 2.996(4) 163.1 . N4 H4C O11 0.91 2.26 3.076(4) 149.4 2_575 O1W H1W O22 0.842(10) 1.836(12) 2.673(3) 172(4) 2_576 O1W H1W S21 0.842(10) 2.76(3) 3.466(3) 143(3) 2_576 O1W H2W O12 0.836(10) 1.874(13) 2.703(3) 171(4) . O1W H2W S11 0.836(10) 2.79(2) 3.535(3) 150(3) . _diffrn_measured_fraction_theta_max 0.897 _diffrn_reflns_theta_full 30.91 _diffrn_measured_fraction_theta_full 0.897 _refine_diff_density_max 1.409 _refine_diff_density_min -1.285 _refine_diff_density_rms 0.122 # Attachment 'rut70.cif' data_rut70 _database_code_depnum_ccdc_archive 'CCDC 604229' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Ru(NH3)4(H2O)(SO2)][CH3C6H4SO3]2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H28 N4 O9 Ru S3' _chemical_formula_weight 593.65 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' S S 0.1246 0.1234 '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 6.670(3) _cell_length_b 13.076(5) _cell_length_c 13.586(5) _cell_angle_alpha 94.352(4) _cell_angle_beta 92.738(4) _cell_angle_gamma 103.482(4) _cell_volume 1146.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 13(2) _cell_measurement_reflns_used 5966 _cell_measurement_theta_min 2.231 _cell_measurement_theta_max 31.1 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.008 _exptl_crystal_size_mid 0.003 _exptl_crystal_size_min 0.003 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 1.009 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9920 _exptl_absorpt_correction_T_max 0.9970 _exptl_absorpt_process_details ; Sortav(Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 13(2) _diffrn_radiation_wavelength 0.68960 _diffrn_radiation_type synchrotron _diffrn_radiation_source ; 'Station 9.8, SRS, Daresbury labs, UK' ; _diffrn_radiation_monochromator 'Si (111)' _diffrn_measurement_device_type 'Bruker APEX 2 diffractometer' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13745 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 31.06 _reflns_number_total 7143 _reflns_number_gt 6315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker SAINT (SAXI, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1995)' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+0.7467P] 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 7143 _refine_ls_number_parameters 292 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0704 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.31096(2) 0.994559(11) 0.245006(10) 0.00448(4) Uani 1 1 d . . . S1 S 0.39823(7) 0.85667(3) 0.19765(3) 0.00589(8) Uani 1 1 d . . . O1 O 0.2936(2) 0.75464(10) 0.22622(10) 0.0105(3) Uani 1 1 d . . . O2 O 0.5619(2) 0.85689(10) 0.13187(10) 0.0089(2) Uani 1 1 d . . . N1 N 0.6014(2) 1.07101(12) 0.31986(11) 0.0074(3) Uani 1 1 d . . . H1A H 0.6665 1.0215 0.3400 0.011 Uiso 1 1 calc R . . H1B H 0.5808 1.1125 0.3735 0.011 Uiso 1 1 calc R . . H1C H 0.6808 1.1116 0.2781 0.011 Uiso 1 1 calc R . . N2 N 0.2070(2) 0.93417(12) 0.37839(11) 0.0075(3) Uani 1 1 d . . . H2A H 0.0856 0.8848 0.3654 0.011 Uiso 1 1 calc R . . H2B H 0.1874 0.9877 0.4209 0.011 Uiso 1 1 calc R . . H2C H 0.3032 0.9040 0.4063 0.011 Uiso 1 1 calc R . . N3 N 0.0070(2) 0.93725(12) 0.17904(11) 0.0077(3) Uani 1 1 d . . . H3A H 0.0114 0.9002 0.1201 0.012 Uiso 1 1 calc R . . H3B H -0.0503 0.9926 0.1689 0.012 Uiso 1 1 calc R . . H3C H -0.0706 0.8944 0.2198 0.012 Uiso 1 1 calc R . . N4 N 0.4044(2) 1.06327(12) 0.11325(11) 0.0076(3) Uani 1 1 d . . . H4A H 0.5448 1.0823 0.1151 0.011 Uiso 1 1 calc R . . H4B H 0.3530 1.1214 0.1079 0.011 Uiso 1 1 calc R . . H4C H 0.3555 1.0156 0.0602 0.011 Uiso 1 1 calc R . . O1W O 0.2276(2) 1.13800(10) 0.28971(10) 0.0074(2) Uani 1 1 d D . . H1W H 0.196(4) 1.1461(19) 0.3481(9) 0.011 Uiso 1 1 d D . . H2W H 0.134(3) 1.1530(19) 0.2549(16) 0.011 Uiso 1 1 d D . . S11 S -0.04168(7) 1.20607(3) 0.08070(3) 0.00541(8) Uani 1 1 d . . . O11 O -0.1717(2) 1.14275(10) -0.00206(10) 0.0095(2) Uani 1 1 d . . . O12 O 0.1789(2) 1.22434(10) 0.06900(10) 0.0093(2) Uani 1 1 d . . . O13 O -0.0968(2) 1.15829(10) 0.17447(10) 0.0081(2) Uani 1 1 d . . . C11 C -0.1036(3) 1.33007(14) 0.09095(13) 0.0064(3) Uani 1 1 d . . . C12 C -0.3035(3) 1.33765(14) 0.06409(13) 0.0080(3) Uani 1 1 d . . . H12 H -0.4033 1.2779 0.0342 0.010 Uiso 1 1 calc R . . C13 C -0.3540(3) 1.43444(14) 0.08189(13) 0.0084(3) Uani 1 1 d . . . H13 H -0.4908 1.4400 0.0652 0.010 Uiso 1 1 calc R . . C14 C -0.2077(3) 1.52385(14) 0.12378(13) 0.0081(3) Uani 1 1 d . . . C15 C -0.0062(3) 1.51454(14) 0.14766(14) 0.0092(3) Uani 1 1 d . . . H15 H 0.0958 1.5749 0.1747 0.011 Uiso 1 1 calc R . . C16 C 0.0457(3) 1.41799(14) 0.13226(13) 0.0082(3) Uani 1 1 d . . . H16 H 0.1818 1.4119 0.1497 0.010 Uiso 1 1 calc R . . C17 C -0.2642(3) 1.62831(15) 0.14270(14) 0.0115(3) Uani 1 1 d . . . H17A H -0.1873 1.6664 0.2029 0.017 Uiso 1 1 calc R . . H17B H -0.4128 1.6161 0.1510 0.017 Uiso 1 1 calc R . . H17C H -0.2293 1.6703 0.0865 0.017 Uiso 1 1 calc R . . S21 S -0.31365(7) 0.81829(3) 0.44579(3) 0.00571(8) Uani 1 1 d . . . O21 O -0.2702(2) 0.86805(10) 0.35345(9) 0.0079(2) Uani 1 1 d . . . O22 O -0.1415(2) 0.85861(10) 0.52118(9) 0.0079(2) Uani 1 1 d . . . O23 O -0.5123(2) 0.82721(10) 0.48162(10) 0.0087(2) Uani 1 1 d . . . C21 C -0.3243(3) 0.68278(14) 0.42002(13) 0.0070(3) Uani 1 1 d . . . C22 C -0.1423(3) 0.64843(14) 0.42719(14) 0.0090(3) Uani 1 1 d . . . H22 H -0.0155 0.6964 0.4499 0.011 Uiso 1 1 calc R . . C23 C -0.1483(3) 0.54321(15) 0.40072(14) 0.0095(3) Uani 1 1 d . . . H23 H -0.0240 0.5197 0.4047 0.011 Uiso 1 1 calc R . . C24 C -0.3336(3) 0.47092(14) 0.36824(13) 0.0086(3) Uani 1 1 d . . . C25 C -0.5144(3) 0.50695(14) 0.36246(14) 0.0093(3) Uani 1 1 d . . . H25 H -0.6417 0.4586 0.3411 0.011 Uiso 1 1 calc R . . C26 C -0.5116(3) 0.61261(15) 0.38746(13) 0.0089(3) Uani 1 1 d . . . H26 H -0.6354 0.6366 0.3824 0.011 Uiso 1 1 calc R . . C27 C -0.3372(3) 0.35671(14) 0.34087(15) 0.0115(3) Uani 1 1 d . . . H27A H -0.2265 0.3522 0.2970 0.017 Uiso 1 1 calc R . . H27B H -0.4709 0.3212 0.3068 0.017 Uiso 1 1 calc R . . H27C H -0.3165 0.3224 0.4010 0.017 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.00408(6) 0.00495(7) 0.00434(7) 0.00021(4) 0.00022(4) 0.00101(4) S1 0.00537(18) 0.00586(18) 0.00629(19) -0.00037(14) -0.00021(14) 0.00146(14) O1 0.0110(6) 0.0071(6) 0.0132(7) 0.0013(5) 0.0013(5) 0.0013(5) O2 0.0072(6) 0.0121(6) 0.0078(6) -0.0006(5) 0.0017(5) 0.0034(5) N1 0.0071(7) 0.0079(7) 0.0074(7) 0.0005(5) -0.0002(5) 0.0020(5) N2 0.0071(7) 0.0085(7) 0.0074(7) 0.0011(5) 0.0015(5) 0.0022(5) N3 0.0069(7) 0.0086(7) 0.0068(7) -0.0003(5) 0.0002(5) 0.0007(5) N4 0.0081(7) 0.0080(7) 0.0071(7) 0.0021(5) 0.0016(5) 0.0022(5) O1W 0.0087(6) 0.0082(6) 0.0065(6) 0.0004(5) 0.0003(5) 0.0049(5) S11 0.00570(18) 0.00577(18) 0.00491(18) 0.00052(14) 0.00034(14) 0.00165(14) O11 0.0114(6) 0.0078(6) 0.0088(6) -0.0023(5) -0.0022(5) 0.0029(5) O12 0.0056(6) 0.0109(6) 0.0121(6) 0.0032(5) 0.0031(5) 0.0024(5) O13 0.0092(6) 0.0093(6) 0.0065(6) 0.0033(5) 0.0019(5) 0.0025(5) C11 0.0078(7) 0.0068(7) 0.0051(7) 0.0011(6) 0.0008(6) 0.0025(6) C12 0.0080(8) 0.0090(8) 0.0064(8) -0.0002(6) 0.0010(6) 0.0013(6) C13 0.0072(7) 0.0106(8) 0.0084(8) 0.0029(6) 0.0018(6) 0.0034(6) C14 0.0112(8) 0.0078(8) 0.0068(8) 0.0014(6) 0.0026(6) 0.0044(6) C15 0.0106(8) 0.0077(8) 0.0083(8) -0.0006(6) 0.0004(6) 0.0005(6) C16 0.0064(7) 0.0092(8) 0.0090(8) 0.0008(6) 0.0019(6) 0.0014(6) C17 0.0165(9) 0.0092(8) 0.0101(8) 0.0011(6) 0.0027(7) 0.0054(7) S21 0.00588(18) 0.00638(18) 0.00507(18) 0.00075(14) 0.00064(14) 0.00177(14) O21 0.0095(6) 0.0086(6) 0.0061(6) 0.0023(4) 0.0018(5) 0.0021(5) O22 0.0081(6) 0.0093(6) 0.0056(6) -0.0007(4) -0.0009(5) 0.0014(5) O23 0.0082(6) 0.0110(6) 0.0085(6) 0.0016(5) 0.0036(5) 0.0047(5) C21 0.0100(8) 0.0055(7) 0.0059(7) 0.0008(6) 0.0014(6) 0.0024(6) C22 0.0086(8) 0.0083(8) 0.0099(8) -0.0002(6) 0.0003(6) 0.0020(6) C23 0.0097(8) 0.0102(8) 0.0097(8) 0.0017(6) 0.0008(6) 0.0045(6) C24 0.0140(8) 0.0065(7) 0.0060(8) 0.0010(6) 0.0028(6) 0.0030(6) C25 0.0085(8) 0.0089(8) 0.0088(8) -0.0005(6) -0.0006(6) -0.0006(6) C26 0.0077(8) 0.0112(8) 0.0084(8) 0.0004(6) 0.0009(6) 0.0033(6) C27 0.0149(9) 0.0067(8) 0.0126(9) 0.0006(6) 0.0022(7) 0.0022(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 Ru S1 2.0863(8) . ? Ru N2 2.1142(16) . ? Ru N4 2.1187(16) . ? Ru N3 2.1193(17) . ? Ru N1 2.1309(16) . ? Ru O1W 2.1312(15) . ? S1 O2 1.4431(14) . ? S1 O1 1.4451(14) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N3 H3C 0.9100 . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N4 H4C 0.9100 . ? O1W H1W 0.836(10) . ? O1W H2W 0.832(10) . ? S11 O12 1.4534(15) . ? S11 O11 1.4604(14) . ? S11 O13 1.4856(14) . ? S11 C11 1.7615(19) . ? C11 C12 1.393(3) . ? C11 C16 1.394(2) . ? C12 C13 1.391(3) . ? C12 H12 0.9500 . ? C13 C14 1.399(3) . ? C13 H13 0.9500 . ? C14 C15 1.402(3) . ? C14 C17 1.507(3) . ? C15 C16 1.389(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? S21 O23 1.4601(14) . ? S21 O21 1.4669(14) . ? S21 O22 1.4729(14) . ? S21 C21 1.7643(19) . ? C21 C22 1.391(3) . ? C21 C26 1.397(3) . ? C22 C23 1.386(3) . ? C22 H22 0.9500 . ? C23 C24 1.398(3) . ? C23 H23 0.9500 . ? C24 C25 1.395(3) . ? C24 C27 1.506(3) . ? C25 C26 1.393(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 S1 Ru N2 92.50(5) . . ? S1 Ru N4 91.27(5) . . ? N2 Ru N4 176.11(6) . . ? S1 Ru N3 92.59(5) . . ? N2 Ru N3 89.05(6) . . ? N4 Ru N3 89.83(6) . . ? S1 Ru N1 95.56(5) . . ? N2 Ru N1 89.77(6) . . ? N4 Ru N1 90.81(6) . . ? N3 Ru N1 171.80(6) . . ? S1 Ru O1W 178.11(4) . . ? N2 Ru O1W 89.33(6) . . ? N4 Ru O1W 86.91(6) . . ? N3 Ru O1W 87.91(6) . . ? N1 Ru O1W 83.96(6) . . ? O2 S1 O1 115.97(8) . . ? O2 S1 Ru 122.10(6) . . ? O1 S1 Ru 121.90(6) . . ? Ru N1 H1A 109.5 . . ? Ru N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? Ru N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Ru N2 H2A 109.5 . . ? Ru N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? Ru N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? Ru N3 H3A 109.5 . . ? Ru N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? Ru N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? Ru N4 H4A 109.5 . . ? Ru N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? Ru N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? Ru O1W H1W 117.2(17) . . ? Ru O1W H2W 116.4(17) . . ? H1W O1W H2W 106(2) . . ? O12 S11 O11 114.50(8) . . ? O12 S11 O13 111.22(8) . . ? O11 S11 O13 109.76(8) . . ? O12 S11 C11 107.56(8) . . ? O11 S11 C11 107.23(8) . . ? O13 S11 C11 106.14(8) . . ? C12 C11 C16 121.13(16) . . ? C12 C11 S11 119.81(14) . . ? C16 C11 S11 118.92(14) . . ? C13 C12 C11 118.70(17) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C12 C13 C14 121.42(17) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C13 C14 C15 118.63(16) . . ? C13 C14 C17 120.95(17) . . ? C15 C14 C17 120.43(17) . . ? C16 C15 C14 120.70(17) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C11 119.39(17) . . ? C15 C16 H16 120.3 . . ? C11 C16 H16 120.3 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O23 S21 O21 112.64(8) . . ? O23 S21 O22 112.43(8) . . ? O21 S21 O22 110.74(8) . . ? O23 S21 C21 107.65(8) . . ? O21 S21 C21 106.95(8) . . ? O22 S21 C21 106.00(8) . . ? C22 C21 C26 120.86(17) . . ? C22 C21 S21 119.06(14) . . ? C26 C21 S21 119.98(14) . . ? C23 C22 C21 119.11(17) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 C24 121.41(17) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C25 C24 C23 118.48(17) . . ? C25 C24 C27 120.94(17) . . ? C23 C24 C27 120.58(17) . . ? C26 C25 C24 121.12(17) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C21 119.02(17) . . ? C25 C26 H26 120.5 . . ? C21 C26 H26 120.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 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 N2 Ru S1 O2 -152.23(8) . . . . ? N4 Ru S1 O2 28.73(8) . . . . ? N3 Ru S1 O2 118.62(8) . . . . ? N1 Ru S1 O2 -62.21(8) . . . . ? N2 Ru S1 O1 29.87(8) . . . . ? N4 Ru S1 O1 -149.17(8) . . . . ? N3 Ru S1 O1 -59.28(9) . . . . ? N1 Ru S1 O1 119.89(9) . . . . ? O12 S11 C11 C12 154.59(14) . . . . ? O11 S11 C11 C12 30.99(17) . . . . ? O13 S11 C11 C12 -86.28(16) . . . . ? O12 S11 C11 C16 -29.68(17) . . . . ? O11 S11 C11 C16 -153.28(14) . . . . ? O13 S11 C11 C16 89.45(15) . . . . ? C16 C11 C12 C13 -1.9(3) . . . . ? S11 C11 C12 C13 173.78(13) . . . . ? C11 C12 C13 C14 1.5(3) . . . . ? C12 C13 C14 C15 0.2(3) . . . . ? C12 C13 C14 C17 179.98(17) . . . . ? C13 C14 C15 C16 -1.5(3) . . . . ? C17 C14 C15 C16 178.69(17) . . . . ? C14 C15 C16 C11 1.2(3) . . . . ? C12 C11 C16 C15 0.6(3) . . . . ? S11 C11 C16 C15 -175.10(14) . . . . ? O23 S21 C21 C22 -151.94(15) . . . . ? O21 S21 C21 C22 86.77(16) . . . . ? O22 S21 C21 C22 -31.42(17) . . . . ? O23 S21 C21 C26 31.68(17) . . . . ? O21 S21 C21 C26 -89.60(16) . . . . ? O22 S21 C21 C26 152.20(14) . . . . ? C26 C21 C22 C23 0.5(3) . . . . ? S21 C21 C22 C23 -175.80(14) . . . . ? C21 C22 C23 C24 -0.8(3) . . . . ? C22 C23 C24 C25 0.3(3) . . . . ? C22 C23 C24 C27 -179.34(17) . . . . ? C23 C24 C25 C26 0.6(3) . . . . ? C27 C24 C25 C26 -179.82(17) . . . . ? C24 C25 C26 C21 -0.8(3) . . . . ? C22 C21 C26 C25 0.3(3) . . . . ? S21 C21 C26 C25 176.58(14) . . . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.762 _refine_diff_density_min -1.125 _refine_diff_density_rms 0.105