Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'E. Alessio' 'Giovanni Birarda' 'Ioannis Bratsos' 'Stephanie Jedner' 'Ennio Zangrando' _publ_contact_author_name 'Enzo Alessio' _publ_contact_author_address ; Dipartimento di Scienze Chimiche University of Trieste Via L. Giorgieri 1 Trieste 34127 ITALY ; _publ_contact_author_email ALESSI@UNITS.IT _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Half-sandwich Ru(II)-[9]aneS3 complexes with dicarboxylate ligands: synthesis, characterization and chemical behavior. ; data_1 _database_code_depnum_ccdc_archive 'CCDC 646389' _audit_creation_method SHELXL-97 _chemical_name_systematic ; dimethylsulfoxide,S-(eta2-oxalate,O,O')-(1,4,7-tritiacyclononane,S,S',S'')- -ruthenium(II) hydrated ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H16 O5 Ru S4, 0.5(H2 O)' _chemical_formula_sum 'C10 H18 O5.50 Ru S4' _chemical_formula_weight 455.55 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' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/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 10.380(3) _cell_length_b 12.439(3) _cell_length_c 12.842(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.72(3) _cell_angle_gamma 90.00 _cell_volume 1596.1(8) _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 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.522 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.4951 _exptl_absorpt_correction_T_max 0.7805 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21723 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 31.06 _reflns_number_total 4996 _reflns_number_gt 3345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (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^)+(0.0637P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4996 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 1.031 _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 Ru Ru 0.46847(3) 0.17879(2) 0.76025(3) 0.03581(10) Uani 1 1 d . . . S1 S 0.54884(11) 0.21575(8) 0.61435(9) 0.0464(2) Uani 1 1 d . . . S2 S 0.68256(12) 0.19584(10) 0.86715(12) 0.0595(3) Uani 1 1 d . . . S3 S 0.44101(11) 0.36482(8) 0.77876(9) 0.0434(2) Uani 1 1 d . . . S4 S 0.49850(11) 0.00066(8) 0.74113(10) 0.0469(3) Uani 1 1 d . . . O1 O 0.3820(4) 0.1553(3) 0.8888(3) 0.0559(8) Uani 1 1 d . . . O2 O 0.2633(3) 0.1667(2) 0.6765(3) 0.0477(7) Uani 1 1 d . . . O3 O 0.0638(4) 0.1474(3) 0.7033(5) 0.0887(15) Uani 1 1 d . . . O4 O 0.6295(4) -0.0313(3) 0.7258(4) 0.0750(11) Uani 1 1 d . . . O5 O 0.1823(6) 0.1502(5) 0.9218(5) 0.117(2) Uani 1 1 d . . . C1 C 0.7322(6) 0.2210(7) 0.6683(7) 0.106(3) Uani 1 1 d . . . H1A H 0.7699 0.1703 0.6273 0.127 Uiso 1 1 calc R . . H1B H 0.7611 0.2921 0.6533 0.127 Uiso 1 1 calc R . . C2 C 0.7895(6) 0.1999(6) 0.7779(6) 0.089(2) Uani 1 1 d . . . H2A H 0.8575 0.2541 0.8052 0.107 Uiso 1 1 calc R . . H2B H 0.8351 0.1312 0.7833 0.107 Uiso 1 1 calc R . . C3 C 0.6948(5) 0.3336(4) 0.9168(4) 0.0598(12) Uani 1 1 d . . . H3A H 0.7255 0.3309 0.9951 0.072 Uiso 1 1 calc R . . H3B H 0.7641 0.3693 0.8919 0.072 Uiso 1 1 calc R . . C4 C 0.5793(10) 0.3994(6) 0.8886(8) 0.144(4) Uani 1 1 d . . . H4A1 H 0.6081 0.4708 0.8741 0.173 Uiso 1 1 calc R . . H4A2 H 0.5464 0.4053 0.9522 0.173 Uiso 1 1 calc R . . C5 C 0.4950(9) 0.4215(5) 0.6714(6) 0.108(3) Uani 1 1 d . . . H5A H 0.4302 0.4762 0.6380 0.130 Uiso 1 1 calc R . . H5B H 0.5787 0.4584 0.7033 0.130 Uiso 1 1 calc R . . C6 C 0.5147(6) 0.3568(4) 0.5886(4) 0.0621(13) Uani 1 1 d . . . H6A H 0.5885 0.3870 0.5654 0.075 Uiso 1 1 calc R . . H6B H 0.4355 0.3626 0.5279 0.075 Uiso 1 1 calc R . . C7 C 0.4731(6) -0.0773(4) 0.8499(5) 0.0699(15) Uani 1 1 d . . . H7A H 0.5353 -0.0551 0.9163 0.105 Uiso 1 1 calc R . . H7B H 0.4869 -0.1520 0.8373 0.105 Uiso 1 1 calc R . . H7C H 0.3833 -0.0670 0.8550 0.105 Uiso 1 1 calc R . . C8 C 0.3739(6) -0.0561(4) 0.6305(5) 0.0656(14) Uani 1 1 d . . . H8A H 0.3771 -0.0214 0.5645 0.098 Uiso 1 1 calc R . . H8B H 0.2870 -0.0457 0.6418 0.098 Uiso 1 1 calc R . . H8C H 0.3905 -0.1316 0.6257 0.098 Uiso 1 1 calc R . . C9 C 0.2530(6) 0.1536(4) 0.8602(5) 0.0621(14) Uani 1 1 d . . . C10 C 0.1856(5) 0.1564(3) 0.7368(5) 0.0556(12) Uani 1 1 d . . . O1W O 0.4288(12) 0.3521(9) 1.0184(11) 0.121(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.03168(16) 0.03736(16) 0.03923(17) 0.00038(12) 0.01105(12) -0.00102(11) S1 0.0461(6) 0.0475(5) 0.0530(6) -0.0038(4) 0.0260(5) -0.0019(4) S2 0.0409(6) 0.0529(6) 0.0713(8) 0.0108(6) -0.0075(6) -0.0052(5) S3 0.0443(6) 0.0403(5) 0.0498(6) -0.0011(4) 0.0199(5) 0.0023(4) S4 0.0405(5) 0.0378(5) 0.0655(7) 0.0009(4) 0.0199(5) 0.0004(4) O1 0.074(2) 0.0579(18) 0.0428(17) 0.0018(13) 0.0284(17) -0.0084(16) O2 0.0310(14) 0.0581(17) 0.0527(18) 0.0022(13) 0.0091(13) -0.0025(12) O3 0.0358(19) 0.073(2) 0.163(5) 0.022(3) 0.036(2) 0.0048(17) O4 0.051(2) 0.0523(18) 0.132(4) 0.000(2) 0.043(2) 0.0106(15) O5 0.138(5) 0.136(4) 0.120(4) -0.038(3) 0.107(4) -0.048(3) C1 0.051(3) 0.151(6) 0.130(6) 0.063(5) 0.049(4) 0.019(4) C2 0.041(3) 0.102(4) 0.122(5) -0.046(4) 0.017(3) -0.001(3) C3 0.058(3) 0.070(3) 0.047(3) -0.010(2) 0.007(2) -0.008(2) C4 0.137(6) 0.080(4) 0.162(7) -0.053(5) -0.049(5) 0.014(4) C5 0.186(7) 0.057(3) 0.120(5) 0.027(3) 0.106(5) 0.035(4) C6 0.081(4) 0.058(3) 0.048(3) 0.010(2) 0.018(3) 0.005(2) C7 0.090(4) 0.042(2) 0.079(4) 0.013(2) 0.024(3) 0.002(2) C8 0.077(4) 0.050(3) 0.071(3) -0.016(2) 0.022(3) -0.007(2) C9 0.082(4) 0.046(2) 0.077(4) -0.014(2) 0.053(3) -0.018(2) C10 0.045(2) 0.0366(19) 0.094(4) 0.006(2) 0.033(3) -0.0007(16) O1W 0.103(9) 0.125(8) 0.135(10) 0.014(7) 0.034(8) 0.010(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 O1 2.102(3) . ? Ru O2 2.115(3) . ? Ru S4 2.2603(12) . ? Ru S2 2.2836(15) . ? Ru S1 2.2946(13) . ? Ru S3 2.3514(12) . ? S1 C6 1.802(5) . ? S1 C1 1.842(7) . ? S2 C2 1.800(7) . ? S2 C3 1.821(5) . ? S3 C5 1.770(6) . ? S3 C4 1.772(8) . ? S4 O4 1.481(3) . ? S4 C7 1.779(5) . ? S4 C8 1.787(5) . ? O1 C9 1.289(7) . ? O2 C10 1.266(6) . ? O3 C10 1.225(6) . ? O5 C9 1.216(6) . ? C1 C2 1.396(10) . ? C3 C4 1.416(10) . ? C5 C6 1.393(8) . ? C9 C10 1.550(8) . ? 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 O1 Ru O2 78.68(14) . . ? O1 Ru S4 92.85(10) . . ? O2 Ru S4 91.40(8) . . ? O1 Ru S2 95.39(11) . . ? O2 Ru S2 173.74(10) . . ? S4 Ru S2 90.91(4) . . ? O1 Ru S1 174.98(10) . . ? O2 Ru S1 97.94(10) . . ? S4 Ru S1 90.94(4) . . ? S2 Ru S1 87.84(6) . . ? O1 Ru S3 88.19(9) . . ? O2 Ru S3 89.34(8) . . ? S4 Ru S3 178.83(4) . . ? S2 Ru S3 88.44(4) . . ? S1 Ru S3 88.06(4) . . ? C6 S1 C1 99.6(3) . . ? C6 S1 Ru 104.37(18) . . ? C1 S1 Ru 105.5(2) . . ? C2 S2 C3 101.5(3) . . ? C2 S2 Ru 106.7(2) . . ? C3 S2 Ru 105.19(18) . . ? C5 S3 C4 99.5(5) . . ? C5 S3 Ru 103.9(2) . . ? C4 S3 Ru 103.0(2) . . ? O4 S4 C7 107.2(3) . . ? O4 S4 C8 106.3(3) . . ? C7 S4 C8 100.4(3) . . ? O4 S4 Ru 115.90(15) . . ? C7 S4 Ru 113.28(18) . . ? C8 S4 Ru 112.46(18) . . ? C9 O1 Ru 114.2(3) . . ? C10 O2 Ru 114.6(3) . . ? C2 C1 S1 119.2(5) . . ? C1 C2 S2 118.6(5) . . ? C4 C3 S2 118.8(4) . . ? C3 C4 S3 120.7(5) . . ? C6 C5 S3 120.5(5) . . ? C5 C6 S1 119.0(4) . . ? O5 C9 O1 125.3(6) . . ? O5 C9 C10 118.7(6) . . ? O1 C9 C10 115.9(4) . . ? O3 C10 O2 124.2(6) . . ? O3 C10 C9 119.6(5) . . ? O2 C10 C9 116.2(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 O1 Ru S1 C6 31.9(11) . . . . ? O2 Ru S1 C6 79.2(2) . . . . ? S4 Ru S1 C6 170.8(2) . . . . ? S2 Ru S1 C6 -98.3(2) . . . . ? S3 Ru S1 C6 -9.8(2) . . . . ? O1 Ru S1 C1 136.3(11) . . . . ? O2 Ru S1 C1 -176.3(3) . . . . ? S4 Ru S1 C1 -84.8(3) . . . . ? S2 Ru S1 C1 6.1(3) . . . . ? S3 Ru S1 C1 94.6(3) . . . . ? O1 Ru S2 C2 172.5(3) . . . . ? O2 Ru S2 C2 -168.7(8) . . . . ? S4 Ru S2 C2 79.6(2) . . . . ? S1 Ru S2 C2 -11.3(2) . . . . ? S3 Ru S2 C2 -99.4(2) . . . . ? O1 Ru S2 C3 -80.1(2) . . . . ? O2 Ru S2 C3 -61.4(8) . . . . ? S4 Ru S2 C3 -173.08(19) . . . . ? S1 Ru S2 C3 96.01(19) . . . . ? S3 Ru S2 C3 7.90(19) . . . . ? O1 Ru S3 C5 -176.0(3) . . . . ? O2 Ru S3 C5 -97.3(3) . . . . ? S4 Ru S3 C5 32(2) . . . . ? S2 Ru S3 C5 88.6(3) . . . . ? S1 Ru S3 C5 0.7(3) . . . . ? O1 Ru S3 C4 80.7(4) . . . . ? O2 Ru S3 C4 159.4(4) . . . . ? S4 Ru S3 C4 -71(2) . . . . ? S2 Ru S3 C4 -14.8(4) . . . . ? S1 Ru S3 C4 -102.7(4) . . . . ? O1 Ru S4 O4 -136.2(2) . . . . ? O2 Ru S4 O4 145.1(2) . . . . ? S2 Ru S4 O4 -40.7(2) . . . . ? S1 Ru S4 O4 47.1(2) . . . . ? S3 Ru S4 O4 16(2) . . . . ? O1 Ru S4 C7 -11.7(3) . . . . ? O2 Ru S4 C7 -90.5(2) . . . . ? S2 Ru S4 C7 83.7(2) . . . . ? S1 Ru S4 C7 171.6(2) . . . . ? S3 Ru S4 C7 140(2) . . . . ? O1 Ru S4 C8 101.2(2) . . . . ? O2 Ru S4 C8 22.5(2) . . . . ? S2 Ru S4 C8 -163.4(2) . . . . ? S1 Ru S4 C8 -75.5(2) . . . . ? S3 Ru S4 C8 -107(2) . . . . ? O2 Ru O1 C9 -5.2(3) . . . . ? S4 Ru O1 C9 -96.1(3) . . . . ? S2 Ru O1 C9 172.8(3) . . . . ? S1 Ru O1 C9 42.8(13) . . . . ? S3 Ru O1 C9 84.5(3) . . . . ? O1 Ru O2 C10 2.8(3) . . . . ? S4 Ru O2 C10 95.4(3) . . . . ? S2 Ru O2 C10 -16.2(9) . . . . ? S1 Ru O2 C10 -173.4(3) . . . . ? S3 Ru O2 C10 -85.5(3) . . . . ? C6 S1 C1 C2 110.1(7) . . . . ? Ru S1 C1 C2 2.2(8) . . . . ? S1 C1 C2 S2 -12.6(10) . . . . ? C3 S2 C2 C1 -93.4(7) . . . . ? Ru S2 C2 C1 16.5(7) . . . . ? C2 S2 C3 C4 114.1(7) . . . . ? Ru S2 C3 C4 3.0(7) . . . . ? S2 C3 C4 S3 -17.8(11) . . . . ? C5 S3 C4 C3 -84.7(9) . . . . ? Ru S3 C4 C3 22.1(10) . . . . ? C4 S3 C5 C6 118.8(7) . . . . ? Ru S3 C5 C6 12.8(8) . . . . ? S3 C5 C6 S1 -23.8(10) . . . . ? C1 S1 C6 C5 -87.5(7) . . . . ? Ru S1 C6 C5 21.3(6) . . . . ? Ru O1 C9 O5 -173.4(5) . . . . ? Ru O1 C9 C10 6.5(5) . . . . ? Ru O2 C10 O3 -179.5(4) . . . . ? Ru O2 C10 C9 -0.4(4) . . . . ? O5 C9 C10 O3 -5.2(7) . . . . ? O1 C9 C10 O3 174.9(4) . . . . ? O5 C9 C10 O2 175.7(5) . . . . ? O1 C9 C10 O2 -4.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 31.06 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.223 _refine_diff_density_min -1.030 _refine_diff_density_rms 0.147 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 646390' _audit_creation_method SHELXL-97 _chemical_name_systematic ; dimethylsulfoxide,S-malonate,O,O'-(1,4,7-tritiacyclononane,S,S',S'')- -ruthenium(II) hydrated ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H20 O5 Ru S4, H2 O' _chemical_formula_sum 'C11 H22 O6 Ru S4' _chemical_formula_weight 479.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.160(3) _cell_length_b 8.100(3) _cell_length_c 23.357(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.80(2) _cell_angle_gamma 90.00 _cell_volume 1675.5(9) _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 yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 1.457 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5771 _exptl_absorpt_correction_T_max 0.8338 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18668 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 29.61 _reflns_number_total 4298 _reflns_number_gt 3249 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (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^)+(0.0376P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4298 _refine_ls_number_parameters 205 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.925 _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 Ru Ru 0.09343(3) 0.13387(2) 0.377308(10) 0.02964(7) Uani 1 1 d . . . S1 S -0.07506(9) 0.26454(9) 0.30113(3) 0.03670(17) Uani 1 1 d . . . S2 S -0.07638(9) 0.15948(9) 0.43312(3) 0.03767(17) Uani 1 1 d . . . S3 S -0.02509(9) -0.11588(8) 0.34024(3) 0.03473(16) Uani 1 1 d . . . S4 S 0.20617(9) 0.37811(8) 0.41157(3) 0.03461(16) Uani 1 1 d . . . O1 O 0.2412(3) 0.0139(2) 0.44892(9) 0.0395(5) Uani 1 1 d . . . O2 O 0.2550(2) 0.1012(2) 0.32762(9) 0.0372(5) Uani 1 1 d . . . O3 O 0.4566(3) -0.0108(3) 0.30966(11) 0.0489(6) Uani 1 1 d . . . O4 O 0.1190(3) 0.5299(3) 0.39062(11) 0.0496(6) Uani 1 1 d . . . O5 O 0.3991(3) -0.1855(3) 0.48815(11) 0.0555(7) Uani 1 1 d . . . C1 C -0.2429(4) 0.3074(4) 0.32898(16) 0.0472(8) Uani 1 1 d . . . H1A H -0.2900 0.4089 0.3114 0.057 Uiso 1 1 calc R . . H1B H -0.3155 0.2187 0.3170 0.057 Uiso 1 1 calc R . . C2 C -0.2019(4) 0.3231(4) 0.39562(16) 0.0480(8) Uani 1 1 d . . . H2A H -0.2937 0.3211 0.4091 0.058 Uiso 1 1 calc R . . H2B H -0.1534 0.4290 0.4066 0.058 Uiso 1 1 calc R . . C3 C -0.2008(4) -0.0216(4) 0.41625(15) 0.0430(7) Uani 1 1 d . . . H3A H -0.2339 -0.0519 0.4511 0.052 Uiso 1 1 calc R . . H3B H -0.2895 0.0060 0.3850 0.052 Uiso 1 1 calc R . . C4 C -0.1212(4) -0.1660(4) 0.39709(14) 0.0423(7) Uani 1 1 d . . . H4A H -0.1946 -0.2523 0.3823 0.051 Uiso 1 1 calc R . . H4B H -0.0479 -0.2093 0.4314 0.051 Uiso 1 1 calc R . . C5 C -0.1825(4) -0.0571(4) 0.27816(13) 0.0382(7) Uani 1 1 d . . . H5A H -0.2032 -0.1459 0.2493 0.046 Uiso 1 1 calc R . . H5B H -0.2721 -0.0400 0.2923 0.046 Uiso 1 1 calc R . . C6 C -0.1472(4) 0.0982(4) 0.24904(13) 0.0404(7) Uani 1 1 d . . . H6A H -0.2382 0.1358 0.2209 0.048 Uiso 1 1 calc R . . H6B H -0.0731 0.0731 0.2272 0.048 Uiso 1 1 calc R . . C7 C 0.2617(5) 0.3898(4) 0.49010(15) 0.0510(9) Uani 1 1 d . . . H7A H 0.1743 0.3800 0.5054 0.077 Uiso 1 1 calc R . . H7B H 0.3101 0.4940 0.5019 0.077 Uiso 1 1 calc R . . H7C H 0.3309 0.3018 0.5054 0.077 Uiso 1 1 calc R . . C8 C 0.3879(4) 0.4004(4) 0.39863(17) 0.0481(8) Uani 1 1 d . . . H8A H 0.3793 0.3970 0.3568 0.072 Uiso 1 1 calc R . . H8B H 0.4519 0.3120 0.4177 0.072 Uiso 1 1 calc R . . H8C H 0.4307 0.5041 0.4143 0.072 Uiso 1 1 calc R . . C9 C 0.3364(4) -0.0988(4) 0.44563(14) 0.0376(7) Uani 1 1 d . . . C10 C 0.3684(4) -0.1361(4) 0.38602(15) 0.0440(8) Uani 1 1 d . . . H10A H 0.2994 -0.2234 0.3679 0.053 Uiso 1 1 calc R . . H10B H 0.4692 -0.1827 0.3945 0.053 Uiso 1 1 calc R . . C11 C 0.3603(4) -0.0048(3) 0.33848(14) 0.0358(6) Uani 1 1 d . . . O1W O 0.4501(4) 0.1509(3) 0.20069(14) 0.0637(8) Uani 1 1 d D . . H1W H 0.477(6) 0.247(3) 0.201(2) 0.096 Uiso 1 1 d D . . H2W H 0.448(6) 0.116(5) 0.2344(12) 0.096 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 Ru 0.02853(13) 0.03187(12) 0.02853(12) 0.00122(8) 0.00731(8) 0.00166(8) S1 0.0368(4) 0.0369(4) 0.0344(4) 0.0045(3) 0.0053(3) 0.0037(3) S2 0.0337(4) 0.0475(4) 0.0335(4) -0.0054(3) 0.0116(3) -0.0020(3) S3 0.0371(4) 0.0334(3) 0.0332(4) -0.0005(3) 0.0081(3) -0.0003(3) S4 0.0331(4) 0.0335(4) 0.0352(4) 0.0011(3) 0.0051(3) -0.0006(3) O1 0.0416(14) 0.0443(11) 0.0314(11) 0.0032(8) 0.0070(10) 0.0087(9) O2 0.0345(13) 0.0427(11) 0.0372(11) 0.0035(8) 0.0144(9) 0.0065(9) O3 0.0445(16) 0.0571(14) 0.0529(15) 0.0077(10) 0.0268(12) 0.0103(11) O4 0.0450(15) 0.0343(11) 0.0616(16) 0.0016(9) -0.0010(12) 0.0053(9) O5 0.0588(18) 0.0578(14) 0.0454(15) 0.0143(11) 0.0050(12) 0.0182(12) C1 0.0313(19) 0.0513(18) 0.055(2) -0.0035(15) 0.0046(15) 0.0122(13) C2 0.038(2) 0.0526(18) 0.055(2) -0.0115(15) 0.0150(16) 0.0076(14) C3 0.042(2) 0.0523(18) 0.0376(17) 0.0006(13) 0.0154(14) -0.0091(14) C4 0.044(2) 0.0455(17) 0.0370(17) 0.0066(12) 0.0103(14) -0.0087(13) C5 0.0360(18) 0.0439(16) 0.0331(16) -0.0049(12) 0.0063(13) -0.0044(12) C6 0.045(2) 0.0476(16) 0.0263(14) -0.0020(12) 0.0040(13) -0.0020(13) C7 0.063(3) 0.0493(19) 0.0376(18) -0.0055(14) 0.0073(16) -0.0108(16) C8 0.035(2) 0.0517(19) 0.056(2) 0.0059(15) 0.0085(16) -0.0070(14) C9 0.0376(18) 0.0370(15) 0.0364(16) 0.0030(11) 0.0063(13) -0.0005(12) C10 0.045(2) 0.0441(18) 0.0479(19) 0.0084(13) 0.0213(15) 0.0123(14) C11 0.0340(18) 0.0362(15) 0.0386(16) -0.0046(11) 0.0121(13) -0.0001(11) O1W 0.080(2) 0.0549(16) 0.0576(18) 0.0019(13) 0.0204(16) -0.0145(14) _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 O1 2.102(2) . ? Ru O2 2.118(2) . ? Ru S2 2.2798(10) . ? Ru S4 2.2800(10) . ? Ru S1 2.2946(9) . ? Ru S3 2.3539(10) . ? S1 C6 1.823(3) . ? S1 C1 1.849(4) . ? S2 C2 1.825(4) . ? S2 C3 1.838(3) . ? S3 C4 1.817(3) . ? S3 C5 1.827(3) . ? S4 O4 1.480(2) . ? S4 C8 1.775(4) . ? S4 C7 1.776(3) . ? O1 C9 1.278(4) . ? O2 C11 1.268(3) . ? O3 C11 1.240(4) . ? O5 C9 1.232(4) . ? C1 C2 1.510(5) . ? C3 C4 1.505(5) . ? C5 C6 1.504(4) . ? C9 C10 1.525(4) . ? C10 C11 1.525(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru O2 88.87(9) . . ? O1 Ru S2 88.96(7) . . ? O2 Ru S2 177.58(6) . . ? O1 Ru S4 88.85(6) . . ? O2 Ru S4 89.06(6) . . ? S2 Ru S4 91.97(3) . . ? O1 Ru S1 177.76(6) . . ? O2 Ru S1 93.35(6) . . ? S2 Ru S1 88.82(4) . . ? S4 Ru S1 91.52(4) . . ? O1 Ru S3 92.18(6) . . ? O2 Ru S3 90.70(6) . . ? S2 Ru S3 88.31(3) . . ? S4 Ru S3 178.93(3) . . ? S1 Ru S3 87.45(4) . . ? C6 S1 C1 100.44(16) . . ? C6 S1 Ru 103.54(11) . . ? C1 S1 Ru 105.58(12) . . ? C2 S2 C3 101.33(17) . . ? C2 S2 Ru 103.29(12) . . ? C3 S2 Ru 106.33(11) . . ? C4 S3 C5 101.93(16) . . ? C4 S3 Ru 100.79(11) . . ? C5 S3 Ru 105.32(10) . . ? O4 S4 C8 108.02(16) . . ? O4 S4 C7 106.57(16) . . ? C8 S4 C7 97.85(19) . . ? O4 S4 Ru 116.57(10) . . ? C8 S4 Ru 112.87(12) . . ? C7 S4 Ru 113.17(11) . . ? C9 O1 Ru 126.36(19) . . ? C11 O2 Ru 125.27(19) . . ? C2 C1 S1 111.6(2) . . ? C1 C2 S2 113.2(2) . . ? C4 C3 S2 111.3(2) . . ? C3 C4 S3 113.9(2) . . ? C6 C5 S3 111.1(2) . . ? C5 C6 S1 113.6(2) . . ? O5 C9 O1 122.9(3) . . ? O5 C9 C10 117.7(3) . . ? O1 C9 C10 119.3(3) . . ? C9 C10 C11 122.8(2) . . ? O3 C11 O2 121.9(3) . . ? O3 C11 C10 117.3(3) . . ? O2 C11 C10 120.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ru S1 C6 -98.4(16) . . . . ? O2 Ru S1 C6 72.81(13) . . . . ? S2 Ru S1 C6 -106.11(12) . . . . ? S4 Ru S1 C6 161.96(12) . . . . ? S3 Ru S1 C6 -17.74(12) . . . . ? O1 Ru S1 C1 6.8(16) . . . . ? O2 Ru S1 C1 177.92(13) . . . . ? S2 Ru S1 C1 -1.00(12) . . . . ? S4 Ru S1 C1 -92.94(12) . . . . ? S3 Ru S1 C1 87.37(12) . . . . ? O1 Ru S2 C2 161.09(13) . . . . ? O2 Ru S2 C2 -172.7(15) . . . . ? S4 Ru S2 C2 72.28(12) . . . . ? S1 Ru S2 C2 -19.21(12) . . . . ? S3 Ru S2 C2 -106.69(12) . . . . ? O1 Ru S2 C3 -92.67(13) . . . . ? O2 Ru S2 C3 -66.4(15) . . . . ? S4 Ru S2 C3 178.51(12) . . . . ? S1 Ru S2 C3 87.03(12) . . . . ? S3 Ru S2 C3 -0.46(12) . . . . ? O1 Ru S3 C4 68.59(13) . . . . ? O2 Ru S3 C4 157.49(13) . . . . ? S2 Ru S3 C4 -20.30(12) . . . . ? S4 Ru S3 C4 -125.6(16) . . . . ? S1 Ru S3 C4 -109.19(12) . . . . ? O1 Ru S3 C5 174.29(13) . . . . ? O2 Ru S3 C5 -96.82(13) . . . . ? S2 Ru S3 C5 85.39(12) . . . . ? S4 Ru S3 C5 -19.9(17) . . . . ? S1 Ru S3 C5 -3.50(11) . . . . ? O1 Ru S4 O4 -159.91(14) . . . . ? O2 Ru S4 O4 111.21(14) . . . . ? S2 Ru S4 O4 -70.99(13) . . . . ? S1 Ru S4 O4 17.88(13) . . . . ? S3 Ru S4 O4 34.3(17) . . . . ? O1 Ru S4 C8 74.19(15) . . . . ? O2 Ru S4 C8 -14.70(14) . . . . ? S2 Ru S4 C8 163.11(13) . . . . ? S1 Ru S4 C8 -108.02(13) . . . . ? S3 Ru S4 C8 -91.6(17) . . . . ? O1 Ru S4 C7 -35.79(16) . . . . ? O2 Ru S4 C7 -124.67(16) . . . . ? S2 Ru S4 C7 53.13(15) . . . . ? S1 Ru S4 C7 142.00(15) . . . . ? S3 Ru S4 C7 158.4(16) . . . . ? O2 Ru O1 C9 -30.5(2) . . . . ? S2 Ru O1 C9 148.4(2) . . . . ? S4 Ru O1 C9 -119.6(2) . . . . ? S1 Ru O1 C9 140.6(15) . . . . ? S3 Ru O1 C9 60.1(2) . . . . ? O1 Ru O2 C11 20.7(2) . . . . ? S2 Ru O2 C11 -5.5(17) . . . . ? S4 Ru O2 C11 109.6(2) . . . . ? S1 Ru O2 C11 -158.9(2) . . . . ? S3 Ru O2 C11 -71.4(2) . . . . ? C6 S1 C1 C2 134.1(2) . . . . ? Ru S1 C1 C2 26.7(3) . . . . ? S1 C1 C2 S2 -46.3(3) . . . . ? C3 S2 C2 C1 -67.6(3) . . . . ? Ru S2 C2 C1 42.4(3) . . . . ? C2 S2 C3 C4 134.8(2) . . . . ? Ru S2 C3 C4 27.2(2) . . . . ? S2 C3 C4 S3 -49.0(3) . . . . ? C5 S3 C4 C3 -63.8(3) . . . . ? Ru S3 C4 C3 44.5(3) . . . . ? C4 S3 C5 C6 134.8(2) . . . . ? Ru S3 C5 C6 29.9(2) . . . . ? S3 C5 C6 S1 -49.2(3) . . . . ? C1 S1 C6 C5 -65.9(3) . . . . ? Ru S1 C6 C5 43.1(3) . . . . ? Ru O1 C9 O5 -165.9(3) . . . . ? Ru O1 C9 C10 10.4(4) . . . . ? O5 C9 C10 C11 -152.2(3) . . . . ? O1 C9 C10 C11 31.3(5) . . . . ? Ru O2 C11 O3 -175.6(2) . . . . ? Ru O2 C11 C10 7.4(4) . . . . ? C9 C10 C11 O3 141.5(3) . . . . ? C9 C10 C11 O2 -41.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 29.61 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 0.582 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.098 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 646391' _audit_creation_method SHELXL-97 _chemical_name_systematic ; dimethylsulfoxide,S-methylmalonate,O,O'-(1,4,7-tritiacyclononane,S,S',S'')- -ruthenium(II) potassium triflate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H22 O5 Ru S4, K 1+, S O3 C F3 1-' _chemical_formula_sum 'C13 H22 F3 K O8 Ru S5' _chemical_formula_weight 663.78 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' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 10.247(3) _cell_length_b 10.176(3) _cell_length_c 12.723(4) _cell_angle_alpha 108.11(2) _cell_angle_beta 103.24(3) _cell_angle_gamma 101.69(3) _cell_volume 1172.5(6) _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 yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.880 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 1.352 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.1961 _exptl_absorpt_correction_T_max 0.7913 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13538 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.88 _reflns_number_total 5030 _reflns_number_gt 3802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (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^)+(0.1011P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5030 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1427 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.00061(3) 0.64607(4) 0.27709(3) 0.04778(14) Uani 1 1 d . . . S1 S -0.14202(11) 0.54728(12) 0.08795(9) 0.0532(3) Uani 1 1 d . . . S2 S -0.19465(11) 0.61665(13) 0.33495(10) 0.0578(3) Uani 1 1 d . . . S3 S -0.00307(12) 0.40944(12) 0.26456(10) 0.0545(3) Uani 1 1 d . . . S4 S -0.00579(12) 0.87358(12) 0.28995(10) 0.0557(3) Uani 1 1 d . . . O1 O 0.1363(3) 0.7362(3) 0.4503(2) 0.0565(7) Uani 1 1 d . . . O2 O 0.1798(3) 0.6814(3) 0.2220(3) 0.0554(7) Uani 1 1 d . . . O3 O 0.4044(3) 0.7282(4) 0.2414(3) 0.0692(9) Uani 1 1 d . . . O4 O -0.1378(4) 0.9079(4) 0.2981(3) 0.0724(9) Uani 1 1 d . . . O5 O 0.3467(4) 0.8473(5) 0.5738(3) 0.0811(11) Uani 1 1 d . . . C1 C -0.3106(5) 0.5680(6) 0.0996(4) 0.0633(11) Uani 1 1 d . . . H1A H -0.3101 0.6665 0.1092 0.076 Uiso 1 1 calc R . . H1B H -0.3831 0.5039 0.0273 0.076 Uiso 1 1 calc R . . C2 C -0.3478(5) 0.5361(6) 0.1988(4) 0.0654(12) Uani 1 1 d . . . H2A H -0.3800 0.4322 0.1774 0.079 Uiso 1 1 calc R . . H2B H -0.4239 0.5747 0.2130 0.079 Uiso 1 1 calc R . . C3 C -0.1976(5) 0.4629(6) 0.3803(4) 0.0651(12) Uani 1 1 d . . . H3A H -0.1322 0.4968 0.4583 0.078 Uiso 1 1 calc R . . H3B H -0.2907 0.4255 0.3840 0.078 Uiso 1 1 calc R . . C4 C -0.1609(5) 0.3406(5) 0.3018(4) 0.0635(11) Uani 1 1 d . . . H4A H -0.2394 0.2876 0.2309 0.076 Uiso 1 1 calc R . . H4B H -0.1439 0.2744 0.3405 0.076 Uiso 1 1 calc R . . C5 C -0.0612(5) 0.3124(5) 0.1067(4) 0.0592(10) Uani 1 1 d . . . H5A H 0.0168 0.3347 0.0777 0.071 Uiso 1 1 calc R . . H5B H -0.0882 0.2091 0.0898 0.071 Uiso 1 1 calc R . . C6 C -0.1829(5) 0.3498(5) 0.0435(4) 0.0591(10) Uani 1 1 d . . . H6A H -0.2664 0.3123 0.0614 0.071 Uiso 1 1 calc R . . H6B H -0.2013 0.3055 -0.0399 0.071 Uiso 1 1 calc R . . C7 C 0.1334(7) 1.0126(6) 0.4077(5) 0.0828(16) Uani 1 1 d . . . H7A H 0.1276 1.0045 0.4798 0.124 Uiso 1 1 calc R . . H7B H 0.1259 1.1054 0.4084 0.124 Uiso 1 1 calc R . . H7C H 0.2217 1.0029 0.3983 0.124 Uiso 1 1 calc R . . C8 C 0.0298(6) 0.9116(6) 0.1702(5) 0.0767(14) Uani 1 1 d . . . H8A H -0.0392 0.8431 0.0989 0.115 Uiso 1 1 calc R . . H8B H 0.1214 0.9045 0.1688 0.115 Uiso 1 1 calc R . . H8C H 0.0262 1.0077 0.1782 0.115 Uiso 1 1 calc R . . C9 C 0.2712(5) 0.7635(5) 0.4786(4) 0.0590(10) Uani 1 1 d . . . C10 C 0.3340(5) 0.6722(6) 0.3941(4) 0.0595(11) Uani 1 1 d . . . H10 H 0.2832 0.5707 0.3739 0.071 Uiso 1 1 calc R . . C11 C 0.3075(4) 0.6990(5) 0.2788(4) 0.0535(9) Uani 1 1 d . . . C12 C 0.4854(6) 0.6902(9) 0.4495(5) 0.096(2) Uani 1 1 d . . . H12A H 0.5199 0.6319 0.3936 0.143 Uiso 1 1 calc R . . H12B H 0.4948 0.6603 0.5146 0.143 Uiso 1 1 calc R . . H12C H 0.5385 0.7900 0.4757 0.143 Uiso 1 1 calc R . . S20 S 0.37968(15) 0.11267(15) 0.07233(12) 0.0686(3) Uani 1 1 d . . . O6 O 0.3484(8) -0.0082(6) 0.1023(7) 0.142(2) Uani 1 1 d . . . O7 O 0.3214(15) 0.1047(14) -0.0307(6) 0.288(8) Uani 1 1 d . . . O8 O 0.5216(7) 0.1690(7) 0.1139(9) 0.201(4) Uani 1 1 d . . . C20 C 0.3162(7) 0.2406(8) 0.1657(6) 0.0846(17) Uani 1 1 d . . . F1 F 0.1854(6) 0.1913(6) 0.1445(8) 0.190(3) Uani 1 1 d . . . F2 F 0.3233(6) 0.3591(4) 0.1417(5) 0.1413(19) Uani 1 1 d . . . F3 F 0.3805(12) 0.2823(11) 0.2661(4) 0.286(6) Uani 1 1 d . . . K1 K 0.59438(11) 0.93991(12) 0.22843(10) 0.0634(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.04139(19) 0.0523(2) 0.0451(2) 0.01472(15) 0.01234(14) 0.01151(14) S1 0.0481(5) 0.0581(6) 0.0472(5) 0.0172(5) 0.0099(4) 0.0126(4) S2 0.0473(6) 0.0653(7) 0.0594(6) 0.0196(5) 0.0207(5) 0.0151(5) S3 0.0506(6) 0.0572(6) 0.0544(6) 0.0218(5) 0.0136(5) 0.0155(5) S4 0.0512(6) 0.0547(6) 0.0571(6) 0.0171(5) 0.0156(5) 0.0150(5) O1 0.0466(16) 0.0681(19) 0.0482(15) 0.0158(14) 0.0126(13) 0.0152(14) O2 0.0447(15) 0.0685(19) 0.0499(15) 0.0212(14) 0.0134(12) 0.0135(13) O3 0.0508(18) 0.085(2) 0.076(2) 0.0342(19) 0.0259(16) 0.0159(16) O4 0.066(2) 0.077(2) 0.084(2) 0.0320(19) 0.0293(18) 0.0331(18) O5 0.063(2) 0.092(3) 0.0535(18) 0.0024(18) 0.0006(16) 0.0096(19) C1 0.044(2) 0.073(3) 0.065(3) 0.025(2) 0.004(2) 0.017(2) C2 0.042(2) 0.075(3) 0.071(3) 0.019(2) 0.012(2) 0.018(2) C3 0.063(3) 0.082(3) 0.059(3) 0.034(3) 0.025(2) 0.019(2) C4 0.062(3) 0.065(3) 0.066(3) 0.031(2) 0.022(2) 0.012(2) C5 0.070(3) 0.052(2) 0.052(2) 0.0152(19) 0.021(2) 0.017(2) C6 0.056(2) 0.056(2) 0.051(2) 0.0093(19) 0.0114(19) 0.011(2) C7 0.082(4) 0.057(3) 0.081(4) 0.009(3) 0.004(3) 0.011(3) C8 0.082(4) 0.071(3) 0.082(4) 0.032(3) 0.030(3) 0.022(3) C9 0.057(3) 0.068(3) 0.046(2) 0.017(2) 0.0142(19) 0.014(2) C10 0.048(2) 0.074(3) 0.051(2) 0.019(2) 0.0126(19) 0.018(2) C11 0.046(2) 0.055(2) 0.055(2) 0.0167(19) 0.0170(18) 0.0122(18) C12 0.065(3) 0.155(6) 0.069(3) 0.036(4) 0.016(3) 0.053(4) S20 0.0671(8) 0.0680(8) 0.0679(7) 0.0223(6) 0.0182(6) 0.0228(6) O6 0.180(6) 0.106(4) 0.203(6) 0.080(4) 0.114(5) 0.078(4) O7 0.481(18) 0.444(16) 0.125(5) 0.148(8) 0.146(8) 0.404(16) O8 0.098(4) 0.107(4) 0.337(11) -0.008(6) 0.104(6) 0.007(3) C20 0.081(4) 0.109(5) 0.090(4) 0.047(4) 0.044(3) 0.047(4) F1 0.161(5) 0.126(4) 0.386(10) 0.128(5) 0.197(7) 0.081(4) F2 0.161(4) 0.074(3) 0.216(6) 0.062(3) 0.088(4) 0.045(3) F3 0.430(13) 0.395(12) 0.068(3) 0.025(5) 0.039(5) 0.339(12) K1 0.0585(6) 0.0628(6) 0.0630(6) 0.0178(5) 0.0188(5) 0.0149(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 Ru O1 2.110(3) . ? Ru O2 2.115(3) . ? Ru S2 2.2812(13) . ? Ru S4 2.2851(14) . ? Ru S1 2.2863(15) . ? Ru S3 2.3552(14) . ? S1 C1 1.815(5) . ? S1 C6 1.838(5) . ? S2 C3 1.826(5) . ? S2 C2 1.867(5) . ? S3 C5 1.828(4) . ? S3 C4 1.852(5) . ? S4 O4 1.482(4) . ? S4 C7 1.779(6) . ? S4 C8 1.780(6) . ? O1 C9 1.293(5) . ? O2 C11 1.288(5) . ? O3 C11 1.219(5) . ? O3 K1 2.670(4) . ? O4 K1 2.801(4) 1_455 ? O5 C9 1.206(5) . ? O5 K1 2.603(4) 2_676 ? C1 C2 1.505(7) . ? C3 C4 1.509(7) . ? C5 C6 1.507(7) . ? C9 C10 1.539(6) . ? C10 C12 1.497(7) . ? C10 C11 1.548(6) . ? S20 O7 1.280(7) . ? S20 O8 1.358(7) . ? S20 O6 1.396(6) . ? S20 C20 1.807(6) . ? S20 K1 3.689(2) 1_545 ? S20 K1 3.775(2) 2_665 ? O6 K1 2.901(7) 1_545 ? O7 K1 2.779(8) 2_665 ? O8 K1 3.229(10) 1_545 ? C20 F3 1.188(8) . ? C20 F1 1.264(8) . ? C20 F2 1.326(8) . ? K1 O5 2.603(4) 2_676 ? K1 O7 2.779(8) 2_665 ? K1 O4 2.801(4) 1_655 ? K1 O6 2.901(7) 1_565 ? K1 O8 3.229(10) 1_565 ? K1 S20 3.689(2) 1_565 ? K1 S20 3.775(2) 2_665 ? 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 O1 Ru O2 88.14(12) . . ? O1 Ru S2 92.47(9) . . ? O2 Ru S2 177.46(9) . . ? O1 Ru S4 88.78(10) . . ? O2 Ru S4 88.25(9) . . ? S2 Ru S4 89.29(5) . . ? O1 Ru S1 178.64(8) . . ? O2 Ru S1 90.58(9) . . ? S2 Ru S1 88.82(5) . . ? S4 Ru S1 91.67(5) . . ? O1 Ru S3 91.89(10) . . ? O2 Ru S3 94.26(9) . . ? S2 Ru S3 88.19(5) . . ? S4 Ru S3 177.42(4) . . ? S1 Ru S3 87.72(5) . . ? C1 S1 C6 99.5(2) . . ? C1 S1 Ru 103.47(17) . . ? C6 S1 Ru 106.79(16) . . ? C3 S2 C2 101.4(2) . . ? C3 S2 Ru 103.89(17) . . ? C2 S2 Ru 106.06(17) . . ? C5 S3 C4 101.5(2) . . ? C5 S3 Ru 101.14(15) . . ? C4 S3 Ru 105.18(17) . . ? O4 S4 C7 107.0(3) . . ? O4 S4 C8 106.8(3) . . ? C7 S4 C8 100.3(3) . . ? O4 S4 Ru 116.54(16) . . ? C7 S4 Ru 113.1(2) . . ? C8 S4 Ru 111.6(2) . . ? C9 O1 Ru 124.1(3) . . ? C11 O2 Ru 127.6(3) . . ? C11 O3 K1 145.6(3) . . ? S4 O4 K1 159.7(2) . 1_455 ? C9 O5 K1 154.1(4) . 2_676 ? C2 C1 S1 114.3(3) . . ? C1 C2 S2 111.7(3) . . ? C4 C3 S2 114.7(3) . . ? C3 C4 S3 111.2(3) . . ? C6 C5 S3 113.2(3) . . ? C5 C6 S1 109.8(3) . . ? O5 C9 O1 121.4(4) . . ? O5 C9 C10 119.5(4) . . ? O1 C9 C10 118.6(4) . . ? C12 C10 C9 112.5(4) . . ? C12 C10 C11 112.6(4) . . ? C9 C10 C11 111.6(4) . . ? O3 C11 O2 122.0(4) . . ? O3 C11 C10 120.3(4) . . ? O2 C11 C10 117.7(4) . . ? O7 S20 O8 115.9(8) . . ? O7 S20 O6 120.2(7) . . ? O8 S20 O6 106.0(5) . . ? O7 S20 C20 105.0(4) . . ? O8 S20 C20 104.7(4) . . ? O6 S20 C20 103.2(3) . . ? O7 S20 K1 141.3(3) . 1_545 ? O8 S20 K1 59.9(4) . 1_545 ? O6 S20 K1 46.1(3) . 1_545 ? C20 S20 K1 113.2(2) . 1_545 ? O7 S20 K1 32.3(5) . 2_665 ? O8 S20 K1 87.8(5) . 2_665 ? O6 S20 K1 119.0(3) . 2_665 ? C20 S20 K1 130.8(2) . 2_665 ? K1 S20 K1 114.13(5) 1_545 2_665 ? S20 O6 K1 113.6(4) . 1_545 ? S20 O7 K1 133.4(7) . 2_665 ? S20 O8 K1 98.8(4) . 1_545 ? F3 C20 F1 113.2(8) . . ? F3 C20 F2 105.2(8) . . ? F1 C20 F2 101.1(6) . . ? F3 C20 S20 113.6(5) . . ? F1 C20 S20 110.6(6) . . ? F2 C20 S20 112.4(5) . . ? O5 K1 O3 103.60(14) 2_676 . ? O5 K1 O7 136.1(3) 2_676 2_665 ? O3 K1 O7 120.2(3) . 2_665 ? O5 K1 O4 90.21(13) 2_676 1_655 ? O3 K1 O4 109.71(12) . 1_655 ? O7 K1 O4 76.1(2) 2_665 1_655 ? O5 K1 O6 97.88(17) 2_676 1_565 ? O3 K1 O6 83.40(15) . 1_565 ? O7 K1 O6 87.5(2) 2_665 1_565 ? O4 K1 O6 162.62(15) 1_655 1_565 ? O5 K1 O8 84.80(19) 2_676 1_565 ? O3 K1 O8 124.90(14) . 1_565 ? O7 K1 O8 70.7(2) 2_665 1_565 ? O4 K1 O8 124.82(13) 1_655 1_565 ? O6 K1 O8 41.62(16) 1_565 1_565 ? O5 K1 S20 91.58(10) 2_676 1_565 ? O3 K1 S20 103.64(9) . 1_565 ? O7 K1 S20 78.70(15) 2_665 1_565 ? O4 K1 S20 145.16(9) 1_655 1_565 ? O6 K1 S20 20.29(12) 1_565 1_565 ? O8 K1 S20 21.33(11) 1_565 1_565 ? O5 K1 S20 138.06(11) 2_676 2_665 ? O3 K1 S20 115.53(10) . 2_665 ? O7 K1 S20 14.3(2) 2_665 2_665 ? O4 K1 S20 90.34(9) 1_655 2_665 ? O6 K1 S20 73.36(13) 1_565 2_665 ? O8 K1 S20 61.12(15) 1_565 2_665 ? S20 K1 S20 65.87(5) 1_565 2_665 ? 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 O1 Ru S1 C1 -178(100) . . . . ? O2 Ru S1 C1 -157.7(2) . . . . ? S2 Ru S1 C1 19.81(18) . . . . ? S4 Ru S1 C1 -69.44(18) . . . . ? S3 Ru S1 C1 108.04(18) . . . . ? O1 Ru S1 C6 77(4) . . . . ? O2 Ru S1 C6 97.87(19) . . . . ? S2 Ru S1 C6 -84.60(17) . . . . ? S4 Ru S1 C6 -173.86(17) . . . . ? S3 Ru S1 C6 3.63(17) . . . . ? O1 Ru S2 C3 -74.2(2) . . . . ? O2 Ru S2 C3 -178(39) . . . . ? S4 Ru S2 C3 -162.93(18) . . . . ? S1 Ru S2 C3 105.38(18) . . . . ? S3 Ru S2 C3 17.63(18) . . . . ? O1 Ru S2 C2 179.4(2) . . . . ? O2 Ru S2 C2 75.5(19) . . . . ? S4 Ru S2 C2 90.65(19) . . . . ? S1 Ru S2 C2 -1.04(18) . . . . ? S3 Ru S2 C2 -88.79(19) . . . . ? O1 Ru S3 C5 -160.02(19) . . . . ? O2 Ru S3 C5 -71.75(19) . . . . ? S2 Ru S3 C5 107.56(18) . . . . ? S4 Ru S3 C5 95.1(9) . . . . ? S1 Ru S3 C5 18.67(18) . . . . ? O1 Ru S3 C4 94.65(19) . . . . ? O2 Ru S3 C4 -177.08(18) . . . . ? S2 Ru S3 C4 2.23(17) . . . . ? S4 Ru S3 C4 -10.3(9) . . . . ? S1 Ru S3 C4 -86.66(17) . . . . ? O1 Ru S4 O4 -107.2(2) . . . . ? O2 Ru S4 O4 164.6(2) . . . . ? S2 Ru S4 O4 -14.71(19) . . . . ? S1 Ru S4 O4 74.09(19) . . . . ? S3 Ru S4 O4 -2.2(10) . . . . ? O1 Ru S4 C7 17.4(3) . . . . ? O2 Ru S4 C7 -70.7(3) . . . . ? S2 Ru S4 C7 109.9(3) . . . . ? S1 Ru S4 C7 -161.3(3) . . . . ? S3 Ru S4 C7 122.4(9) . . . . ? O1 Ru S4 C8 129.7(2) . . . . ? O2 Ru S4 C8 41.5(2) . . . . ? S2 Ru S4 C8 -137.8(2) . . . . ? S1 Ru S4 C8 -49.0(2) . . . . ? S3 Ru S4 C8 -125.3(9) . . . . ? O2 Ru O1 C9 -10.9(4) . . . . ? S2 Ru O1 C9 171.6(4) . . . . ? S4 Ru O1 C9 -99.2(4) . . . . ? S1 Ru O1 C9 10(4) . . . . ? S3 Ru O1 C9 83.3(4) . . . . ? O1 Ru O2 C11 20.9(4) . . . . ? S2 Ru O2 C11 124.9(18) . . . . ? S4 Ru O2 C11 109.7(4) . . . . ? S1 Ru O2 C11 -158.6(4) . . . . ? S3 Ru O2 C11 -70.9(4) . . . . ? C7 S4 O4 K1 139.2(7) . . . 1_455 ? C8 S4 O4 K1 32.4(7) . . . 1_455 ? Ru S4 O4 K1 -93.1(6) . . . 1_455 ? C6 S1 C1 C2 68.7(4) . . . . ? Ru S1 C1 C2 -41.3(4) . . . . ? S1 C1 C2 S2 43.1(5) . . . . ? C3 S2 C2 C1 -131.4(4) . . . . ? Ru S2 C2 C1 -23.2(4) . . . . ? C2 S2 C3 C4 68.4(4) . . . . ? Ru S2 C3 C4 -41.5(4) . . . . ? S2 C3 C4 S3 46.1(5) . . . . ? C5 S3 C4 C3 -132.1(4) . . . . ? Ru S3 C4 C3 -27.1(4) . . . . ? C4 S3 C5 C6 62.9(4) . . . . ? Ru S3 C5 C6 -45.3(4) . . . . ? S3 C5 C6 S1 51.9(4) . . . . ? C1 S1 C6 C5 -138.7(3) . . . . ? Ru S1 C6 C5 -31.4(3) . . . . ? K1 O5 C9 O1 -19.8(12) 2_676 . . . ? K1 O5 C9 C10 168.2(6) 2_676 . . . ? Ru O1 C9 O5 160.4(4) . . . . ? Ru O1 C9 C10 -27.5(6) . . . . ? O5 C9 C10 C12 6.2(7) . . . . ? O1 C9 C10 C12 -166.1(5) . . . . ? O5 C9 C10 C11 -121.6(5) . . . . ? O1 C9 C10 C11 66.2(6) . . . . ? K1 O3 C11 O2 87.3(7) . . . . ? K1 O3 C11 C10 -96.6(6) . . . . ? Ru O2 C11 O3 -175.0(3) . . . . ? Ru O2 C11 C10 8.8(6) . . . . ? C12 C10 C11 O3 1.4(7) . . . . ? C9 C10 C11 O3 129.1(5) . . . . ? C12 C10 C11 O2 177.6(5) . . . . ? C9 C10 C11 O2 -54.7(5) . . . . ? O7 S20 O6 K1 133.9(5) . . . 1_545 ? O8 S20 O6 K1 0.1(5) . . . 1_545 ? C20 S20 O6 K1 -109.7(3) . . . 1_545 ? K1 S20 O6 K1 96.6(3) 2_665 . . 1_545 ? O8 S20 O7 K1 32.1(12) . . . 2_665 ? O6 S20 O7 K1 -97.5(12) . . . 2_665 ? C20 S20 O7 K1 147.1(9) . . . 2_665 ? K1 S20 O7 K1 -41.4(19) 1_545 . . 2_665 ? O7 S20 O8 K1 -136.2(5) . . . 1_545 ? O6 S20 O8 K1 0.0(5) . . . 1_545 ? C20 S20 O8 K1 108.6(3) . . . 1_545 ? K1 S20 O8 K1 -119.7(2) 2_665 . . 1_545 ? O7 S20 C20 F3 -166.1(11) . . . . ? O8 S20 C20 F3 -43.5(10) . . . . ? O6 S20 C20 F3 67.3(9) . . . . ? K1 S20 C20 F3 19.7(9) 1_545 . . . ? K1 S20 C20 F3 -143.5(8) 2_665 . . . ? O7 S20 C20 F1 65.4(9) . . . . ? O8 S20 C20 F1 -172.0(7) . . . . ? O6 S20 C20 F1 -61.3(7) . . . . ? K1 S20 C20 F1 -108.9(5) 1_545 . . . ? K1 S20 C20 F1 87.9(6) 2_665 . . . ? O7 S20 C20 F2 -46.8(9) . . . . ? O8 S20 C20 F2 75.8(7) . . . . ? O6 S20 C20 F2 -173.4(6) . . . . ? K1 S20 C20 F2 139.0(4) 1_545 . . . ? K1 S20 C20 F2 -24.2(7) 2_665 . . . ? C11 O3 K1 O5 33.0(6) . . . 2_676 ? C11 O3 K1 O7 -146.8(6) . . . 2_665 ? C11 O3 K1 O4 128.2(5) . . . 1_655 ? C11 O3 K1 O6 -63.6(6) . . . 1_565 ? C11 O3 K1 O8 -60.2(6) . . . 1_565 ? C11 O3 K1 S20 -62.0(6) . . . 1_565 ? C11 O3 K1 S20 -131.5(5) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 0.935 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.116 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 646392' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis[fac-(1,4,7-tritiacyclononane)-(dimethylsulfoxide,S)-ruthenium(II)] -(mu-oxalate) bis(triflate) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H36 O6 Ru2 S8 2+, 2(S O3 C F3 1-)' _chemical_formula_sum 'C20 H36 F6 O12 Ru2 S10' _chemical_formula_weight 1105.23 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 8.386(3) _cell_length_b 10.893(4) _cell_length_c 12.009(4) _cell_angle_alpha 66.32(3) _cell_angle_beta 76.37(3) _cell_angle_gamma 87.55(3) _cell_volume 974.6(6) _cell_formula_units_Z 1 _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 1.883 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 554 _exptl_absorpt_coefficient_mu 1.390 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25340 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.1490 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3319 _reflns_number_gt 1539 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (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^)+(0.0526P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3319 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1509 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.1934 _refine_ls_wR_factor_gt 0.1813 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.85369(13) 0.16281(12) 0.81146(10) 0.0520(4) Uani 1 1 d . . . S1 S 0.5953(4) 0.1728(4) 0.7800(3) 0.0586(9) Uani 1 1 d . . . S2 S 0.9126(4) 0.3683(4) 0.6500(3) 0.0629(10) Uani 1 1 d . . . S3 S 0.7646(4) 0.2693(4) 0.9482(3) 0.0599(10) Uani 1 1 d . . . S4 S 0.9435(5) 0.0628(4) 0.6756(4) 0.0724(12) Uani 1 1 d . . . O1 O 1.0873(9) 0.1435(9) 0.8628(8) 0.057(2) Uani 1 1 d . . . O2 O 0.8095(10) -0.0230(9) 0.9724(8) 0.060(2) Uani 1 1 d . . . O4 O 0.9032(19) 0.1269(16) 0.5522(11) 0.155(7) Uani 1 1 d . . . C1 C 0.6123(16) 0.3012(16) 0.6238(12) 0.072(4) Uani 1 1 d . . . H1A H 0.6552 0.2633 0.5629 0.087 Uiso 1 1 calc R . . H1B H 0.5041 0.3317 0.6143 0.087 Uiso 1 1 calc R . . C2 C 0.7230(17) 0.4185(14) 0.5986(13) 0.068(4) Uani 1 1 d . . . H2A H 0.6648 0.4721 0.6413 0.081 Uiso 1 1 calc R . . H2B H 0.7502 0.4741 0.5095 0.081 Uiso 1 1 calc R . . C3 C 0.9272(17) 0.4770(16) 0.7296(15) 0.082(5) Uani 1 1 d . . . H3A H 1.0333 0.4674 0.7505 0.098 Uiso 1 1 calc R . . H3B H 0.9239 0.5693 0.6717 0.098 Uiso 1 1 calc R . . C4 C 0.797(2) 0.4515(16) 0.8461(15) 0.090(5) Uani 1 1 d . . . H4A H 0.6949 0.4857 0.8241 0.108 Uiso 1 1 calc R . . H4B H 0.8285 0.4991 0.8914 0.108 Uiso 1 1 calc R . . C5 C 0.5438(16) 0.2415(16) 0.9816(14) 0.073(4) Uani 1 1 d . . . H5A H 0.5134 0.1504 1.0434 0.088 Uiso 1 1 calc R . . H5B H 0.4920 0.3017 1.0191 0.088 Uiso 1 1 calc R . . C6 C 0.4763(15) 0.2613(15) 0.8725(13) 0.065(4) Uani 1 1 d . . . H6A H 0.4802 0.3565 0.8200 0.078 Uiso 1 1 calc R . . H6B H 0.3623 0.2276 0.9014 0.078 Uiso 1 1 calc R . . C7 C 1.1577(17) 0.052(2) 0.6435(17) 0.108(6) Uani 1 1 d . . . H7A H 1.2102 0.1402 0.6073 0.161 Uiso 1 1 calc R . . H7B H 1.1902 0.0096 0.5858 0.161 Uiso 1 1 calc R . . H7C H 1.1899 -0.0007 0.7198 0.161 Uiso 1 1 calc R . . C8 C 0.883(2) -0.1110(18) 0.742(2) 0.122(7) Uani 1 1 d . . . H8A H 0.7655 -0.1225 0.7656 0.183 Uiso 1 1 calc R . . H8B H 0.9257 -0.1559 0.8154 0.183 Uiso 1 1 calc R . . H8C H 0.9262 -0.1488 0.6823 0.183 Uiso 1 1 calc R . . C9 C 0.9207(15) -0.0500(14) 1.0335(13) 0.056(3) Uani 1 1 d . . . S5 S 0.3303(5) 0.6250(4) 0.7565(4) 0.0697(11) Uani 1 1 d . . . O5 O 0.1697(12) 0.6775(11) 0.7759(12) 0.102(4) Uani 1 1 d . . . O6 O 0.3581(13) 0.5526(10) 0.6766(9) 0.080(3) Uani 1 1 d . . . O7 O 0.3925(13) 0.5620(11) 0.8665(9) 0.087(3) Uani 1 1 d . . . C10 C 0.470(2) 0.7687(19) 0.6678(16) 0.088(5) Uani 1 1 d . . . F1 F 0.4420(15) 0.8464(11) 0.5567(10) 0.123(4) Uani 1 1 d . . . F2 F 0.6267(13) 0.7360(13) 0.6453(12) 0.147(5) Uani 1 1 d . . . F3 F 0.4615(12) 0.8529(10) 0.7289(9) 0.107(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0560(7) 0.0568(8) 0.0431(7) -0.0192(6) -0.0146(5) 0.0103(5) S1 0.063(2) 0.059(2) 0.059(2) -0.0261(19) -0.0220(17) 0.0093(17) S2 0.063(2) 0.062(3) 0.049(2) -0.0095(19) -0.0125(16) 0.0078(17) S3 0.064(2) 0.067(3) 0.053(2) -0.030(2) -0.0126(17) 0.0077(18) S4 0.085(3) 0.090(3) 0.058(2) -0.044(2) -0.0262(19) 0.035(2) O1 0.047(5) 0.065(6) 0.048(5) -0.010(5) -0.011(4) -0.003(4) O2 0.060(5) 0.055(6) 0.053(6) -0.006(5) -0.021(4) 0.001(4) O4 0.229(14) 0.204(16) 0.089(9) -0.100(10) -0.092(10) 0.158(13) C1 0.070(9) 0.103(13) 0.053(9) -0.034(9) -0.032(7) 0.044(9) C2 0.079(9) 0.055(10) 0.062(9) -0.014(8) -0.022(7) 0.005(8) C3 0.066(9) 0.059(10) 0.108(13) -0.024(10) -0.015(9) 0.010(7) C4 0.108(13) 0.074(12) 0.096(13) -0.049(11) -0.010(10) -0.013(9) C5 0.070(9) 0.081(12) 0.077(11) -0.048(9) -0.007(8) 0.015(8) C6 0.046(8) 0.067(10) 0.082(11) -0.033(8) -0.012(7) 0.016(7) C7 0.076(11) 0.138(18) 0.117(15) -0.073(14) -0.001(10) 0.008(11) C8 0.096(14) 0.093(15) 0.18(2) -0.075(15) -0.011(13) -0.009(11) C9 0.060(8) 0.058(10) 0.048(8) -0.020(8) -0.014(7) -0.002(7) S5 0.076(2) 0.068(3) 0.072(3) -0.033(2) -0.022(2) 0.019(2) O5 0.064(7) 0.100(9) 0.164(12) -0.079(9) -0.025(6) 0.030(6) O6 0.116(8) 0.073(7) 0.071(7) -0.049(6) -0.025(6) 0.023(6) O7 0.125(9) 0.077(8) 0.066(7) -0.026(6) -0.039(6) 0.009(6) C10 0.122(15) 0.093(14) 0.065(11) -0.043(11) -0.035(10) 0.023(11) F1 0.194(11) 0.094(8) 0.084(7) -0.029(6) -0.050(7) -0.002(7) F2 0.089(8) 0.160(12) 0.170(12) -0.062(10) 0.001(7) -0.003(7) F3 0.138(8) 0.094(8) 0.109(8) -0.059(7) -0.031(6) -0.006(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru O2 2.134(9) . ? Ru O1 2.166(8) . ? Ru S2 2.274(4) . ? Ru S1 2.277(3) . ? Ru S4 2.279(4) . ? Ru S3 2.340(4) . ? S1 C1 1.811(14) . ? S1 C6 1.848(13) . ? S2 C3 1.818(16) . ? S2 C2 1.823(13) . ? S3 C5 1.811(13) . ? S3 C4 1.858(16) . ? S4 O4 1.478(11) . ? S4 C7 1.756(15) . ? S4 C8 1.776(18) . ? O1 C9 1.241(14) 2_757 ? O2 C9 1.273(14) . ? C1 C2 1.497(19) . ? C3 C4 1.49(2) . ? C5 C6 1.482(17) . ? C9 O1 1.241(14) 2_757 ? C9 C9 1.59(2) 2_757 ? S5 O7 1.433(10) . ? S5 O6 1.443(9) . ? S5 O5 1.445(9) . ? S5 C10 1.78(2) . ? C10 F1 1.331(17) . ? C10 F2 1.344(19) . ? C10 F3 1.376(18) . ? 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 O2 Ru O1 78.8(3) . . ? O2 Ru S2 174.6(3) . . ? O1 Ru S2 97.2(3) . . ? O2 Ru S1 96.2(2) . . ? O1 Ru S1 173.8(3) . . ? S2 Ru S1 87.55(14) . . ? O2 Ru S4 93.6(3) . . ? O1 Ru S4 92.0(3) . . ? S2 Ru S4 90.08(16) . . ? S1 Ru S4 91.89(14) . . ? O2 Ru S3 87.3(3) . . ? O1 Ru S3 87.6(3) . . ? S2 Ru S3 88.89(14) . . ? S1 Ru S3 88.52(13) . . ? S4 Ru S3 178.88(18) . . ? C1 S1 C6 99.5(6) . . ? C1 S1 Ru 105.1(5) . . ? C6 S1 Ru 106.3(4) . . ? C3 S2 C2 101.7(7) . . ? C3 S2 Ru 102.4(5) . . ? C2 S2 Ru 106.4(5) . . ? C5 S3 C4 102.5(7) . . ? C5 S3 Ru 101.0(5) . . ? C4 S3 Ru 104.6(5) . . ? O4 S4 C7 105.6(8) . . ? O4 S4 C8 109.2(10) . . ? C7 S4 C8 99.0(9) . . ? O4 S4 Ru 116.4(5) . . ? C7 S4 Ru 112.3(6) . . ? C8 S4 Ru 112.7(7) . . ? C9 O1 Ru 111.3(8) 2_757 . ? C9 O2 Ru 114.5(8) . . ? C2 C1 S1 111.6(9) . . ? C1 C2 S2 112.9(9) . . ? C4 C3 S2 115.6(11) . . ? C3 C4 S3 111.2(11) . . ? C6 C5 S3 115.6(10) . . ? C5 C6 S1 110.6(9) . . ? O1 C9 O2 125.9(12) 2_757 . ? O1 C9 C9 120.0(14) 2_757 2_757 ? O2 C9 C9 114.1(15) . 2_757 ? O7 S5 O6 113.6(6) . . ? O7 S5 O5 115.4(7) . . ? O6 S5 O5 116.0(7) . . ? O7 S5 C10 101.6(7) . . ? O6 S5 C10 102.4(7) . . ? O5 S5 C10 105.3(8) . . ? F1 C10 F2 106.0(15) . . ? F1 C10 F3 104.5(14) . . ? F2 C10 F3 106.8(15) . . ? F1 C10 S5 114.7(13) . . ? F2 C10 S5 112.5(13) . . ? F3 C10 S5 111.6(12) . . ? 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 O2 Ru S1 C1 -165.8(6) . . . . ? O1 Ru S1 C1 159(3) . . . . ? S2 Ru S1 C1 18.0(5) . . . . ? S4 Ru S1 C1 -72.0(5) . . . . ? S3 Ru S1 C1 107.0(5) . . . . ? O2 Ru S1 C6 89.3(6) . . . . ? O1 Ru S1 C6 54(3) . . . . ? S2 Ru S1 C6 -86.9(5) . . . . ? S4 Ru S1 C6 -176.9(5) . . . . ? S3 Ru S1 C6 2.1(5) . . . . ? O2 Ru S2 C3 -26(3) . . . . ? O1 Ru S2 C3 -67.6(5) . . . . ? S1 Ru S2 C3 108.5(5) . . . . ? S4 Ru S2 C3 -159.6(5) . . . . ? S3 Ru S2 C3 19.9(5) . . . . ? O2 Ru S2 C2 -132(3) . . . . ? O1 Ru S2 C2 -173.9(6) . . . . ? S1 Ru S2 C2 2.1(5) . . . . ? S4 Ru S2 C2 94.0(5) . . . . ? S3 Ru S2 C2 -86.4(5) . . . . ? O2 Ru S3 C5 -78.3(6) . . . . ? O1 Ru S3 C5 -157.2(6) . . . . ? S2 Ru S3 C5 105.5(5) . . . . ? S1 Ru S3 C5 17.9(5) . . . . ? S4 Ru S3 C5 129(7) . . . . ? O2 Ru S3 C4 175.5(6) . . . . ? O1 Ru S3 C4 96.7(6) . . . . ? S2 Ru S3 C4 -0.6(6) . . . . ? S1 Ru S3 C4 -88.2(6) . . . . ? S4 Ru S3 C4 23(7) . . . . ? O2 Ru S4 O4 145.5(9) . . . . ? O1 Ru S4 O4 -135.6(9) . . . . ? S2 Ru S4 O4 -38.4(9) . . . . ? S1 Ru S4 O4 49.2(9) . . . . ? S3 Ru S4 O4 -62(7) . . . . ? O2 Ru S4 C7 -92.6(7) . . . . ? O1 Ru S4 C7 -13.8(7) . . . . ? S2 Ru S4 C7 83.5(7) . . . . ? S1 Ru S4 C7 171.0(7) . . . . ? S3 Ru S4 C7 60(7) . . . . ? O2 Ru S4 C8 18.2(7) . . . . ? O1 Ru S4 C8 97.1(7) . . . . ? S2 Ru S4 C8 -165.7(7) . . . . ? S1 Ru S4 C8 -78.1(7) . . . . ? S3 Ru S4 C8 171(7) . . . . ? O2 Ru O1 C9 -9.7(9) . . . 2_757 ? S2 Ru O1 C9 166.6(9) . . . 2_757 ? S1 Ru O1 C9 26(3) . . . 2_757 ? S4 Ru O1 C9 -103.1(9) . . . 2_757 ? S3 Ru O1 C9 78.0(9) . . . 2_757 ? O1 Ru O2 C9 9.7(9) . . . . ? S2 Ru O2 C9 -33(3) . . . . ? S1 Ru O2 C9 -166.6(9) . . . . ? S4 Ru O2 C9 101.1(9) . . . . ? S3 Ru O2 C9 -78.4(9) . . . . ? C6 S1 C1 C2 69.5(10) . . . . ? Ru S1 C1 C2 -40.3(10) . . . . ? S1 C1 C2 S2 45.0(13) . . . . ? C3 S2 C2 C1 -134.5(11) . . . . ? Ru S2 C2 C1 -27.7(11) . . . . ? C2 S2 C3 C4 66.3(13) . . . . ? Ru S2 C3 C4 -43.6(13) . . . . ? S2 C3 C4 S3 46.1(16) . . . . ? C5 S3 C4 C3 -129.6(12) . . . . ? Ru S3 C4 C3 -24.5(13) . . . . ? C4 S3 C5 C6 65.1(12) . . . . ? Ru S3 C5 C6 -42.7(12) . . . . ? S3 C5 C6 S1 48.0(14) . . . . ? C1 S1 C6 C5 -136.5(11) . . . . ? Ru S1 C6 C5 -27.6(12) . . . . ? Ru O2 C9 O1 171.1(11) . . . 2_757 ? Ru O2 C9 C9 -8.0(17) . . . 2_757 ? O7 S5 C10 F1 178.7(12) . . . . ? O6 S5 C10 F1 61.1(14) . . . . ? O5 S5 C10 F1 -60.7(14) . . . . ? O7 S5 C10 F2 57.4(13) . . . . ? O6 S5 C10 F2 -60.2(13) . . . . ? O5 S5 C10 F2 178.1(12) . . . . ? O7 S5 C10 F3 -62.6(13) . . . . ? O6 S5 C10 F3 179.8(12) . . . . ? O5 S5 C10 F3 58.0(14) . . . . ? _diffrn_measured_fraction_theta_max 0.815 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.815 _refine_diff_density_max 1.310 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.149 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 646393' _audit_creation_method SHELXL-97 _chemical_name_systematic ; fac-(1,4,7-tritiacyclononane)-(dimethylsulfoxide,S)-ruthenium(II)-(mu-oxalate)- fac-tris(dimethylsulfoxide,S)-(triflate,O)-ruthenium(II) triflate chloroform solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H36 F3 O11 Ru2 S8 1+, C F3 S O3 1-, 0.5(C H Cl3)' _chemical_formula_sum 'C18.50 H36.50 Cl1.50 F6 O14 Ru2 S9' _chemical_formula_weight 1140.83 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P nma' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 16.558(4) _cell_length_b 41.174(7) _cell_length_c 12.341(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8414(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.801 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4568 _exptl_absorpt_coefficient_mu 1.339 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.2978 _exptl_absorpt_correction_T_max 0.9232 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76589 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8178 _reflns_number_gt 4232 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (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^)+(0.1112P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8178 _refine_ls_number_parameters 459 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1805 _refine_ls_wR_factor_gt 0.1681 _refine_ls_goodness_of_fit_ref 0.879 _refine_ls_restrained_S_all 0.887 _refine_ls_shift/su_max 0.002 _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 0.09439(5) 0.627867(15) 0.33225(4) 0.0585(2) Uani 1 1 d . . . S1 S -0.03792(17) 0.62440(6) 0.28220(15) 0.0711(7) Uani 1 1 d . . . S2 S 0.11124(19) 0.66583(6) 0.19944(16) 0.0802(8) Uani 1 1 d . . . S3 S 0.0573(2) 0.66928(6) 0.45189(16) 0.0866(9) Uani 1 1 d . . . C1 C -0.0545(7) 0.6542(3) 0.1693(7) 0.093(3) Uani 1 1 d . . . H12A H -0.0924 0.6452 0.1175 0.111 Uiso 1 1 calc R . . H12B H -0.0777 0.6740 0.1984 0.111 Uiso 1 1 calc R . . C2 C 0.0236(7) 0.6619(3) 0.1133(6) 0.102(4) Uani 1 1 d . . . H11A H 0.0168 0.6821 0.0737 0.122 Uiso 1 1 calc R . . H11B H 0.0342 0.6450 0.0605 0.122 Uiso 1 1 calc R . . C3 C 0.0893(9) 0.7053(2) 0.2640(9) 0.122(5) Uani 1 1 d . . . H16A H 0.1246 0.7217 0.2334 0.146 Uiso 1 1 calc R . . H16B H 0.0341 0.7115 0.2477 0.146 Uiso 1 1 calc R . . C4 C 0.1004(9) 0.7046(2) 0.3837(8) 0.123(5) Uani 1 1 d . . . H15A H 0.0762 0.7240 0.4142 0.148 Uiso 1 1 calc R . . H15B H 0.1577 0.7053 0.3993 0.148 Uiso 1 1 calc R . . C5 C -0.0485(8) 0.6752(2) 0.4329(7) 0.102(4) Uani 1 1 d . . . H14A H -0.0722 0.6815 0.5016 0.122 Uiso 1 1 calc R . . H14B H -0.0564 0.6930 0.3826 0.122 Uiso 1 1 calc R . . C6 C -0.0947(7) 0.6446(3) 0.3890(8) 0.098(4) Uani 1 1 d . . . H13A H -0.1469 0.6512 0.3612 0.118 Uiso 1 1 calc R . . H13B H -0.1037 0.6294 0.4481 0.118 Uiso 1 1 calc R . . S4 S 0.13210(17) 0.58865(6) 0.21252(14) 0.0680(6) Uani 1 1 d . . . O4 O 0.1000(4) 0.59170(16) 0.1015(4) 0.086(2) Uani 1 1 d . . . C7 C 0.2362(8) 0.5837(4) 0.2038(7) 0.121(5) Uani 1 1 d . . . H10A H 0.2602 0.6033 0.1765 0.181 Uiso 1 1 calc R . . H10B H 0.2482 0.5660 0.1557 0.181 Uiso 1 1 calc R . . H10C H 0.2576 0.5790 0.2744 0.181 Uiso 1 1 calc R . . C8 C 0.1041(8) 0.5494(2) 0.2609(8) 0.102(4) Uani 1 1 d . . . H9A H 0.0469 0.5488 0.2735 0.153 Uiso 1 1 calc R . . H9B H 0.1321 0.5450 0.3274 0.153 Uiso 1 1 calc R . . H9C H 0.1183 0.5333 0.2079 0.153 Uiso 1 1 calc R . . O1 O 0.2133(4) 0.63282(13) 0.3961(3) 0.0654(16) Uani 1 1 d . . . O2 O 0.0912(4) 0.59444(12) 0.4687(3) 0.0578(14) Uani 1 1 d . . . C9 C 0.2201(6) 0.62053(17) 0.4892(5) 0.056(2) Uani 1 1 d . . . C10 C 0.1515(6) 0.59823(17) 0.5279(5) 0.059(2) Uani 1 1 d . . . O8 O 0.1625(4) 0.58416(12) 0.6190(3) 0.0602(15) Uani 1 1 d . . . O9 O 0.2793(4) 0.62516(12) 0.5496(3) 0.0599(14) Uani 1 1 d . . . Ru2 Ru 0.26899(4) 0.600086(14) 0.69929(4) 0.05195(19) Uani 1 1 d . . . S5 S 0.38844(15) 0.61885(5) 0.75882(14) 0.0618(6) Uani 1 1 d . . . O5 O 0.3901(4) 0.64401(16) 0.8426(4) 0.0803(19) Uani 1 1 d . . . S6 S 0.24926(15) 0.56887(5) 0.84582(13) 0.0608(6) Uani 1 1 d . . . O6 O 0.2859(4) 0.57874(15) 0.9495(3) 0.0752(19) Uani 1 1 d . . . S7 S 0.19973(17) 0.64215(5) 0.76873(15) 0.0635(6) Uani 1 1 d . . . O7 O 0.1130(4) 0.64055(16) 0.7431(5) 0.086(2) Uani 1 1 d . . . C11 C 0.4417(6) 0.6349(3) 0.6430(7) 0.084(3) Uani 1 1 d . . . H5A H 0.4074 0.6499 0.6051 0.126 Uiso 1 1 calc R . . H5B H 0.4563 0.6174 0.5954 0.126 Uiso 1 1 calc R . . H5C H 0.4896 0.6459 0.6669 0.126 Uiso 1 1 calc R . . C12 C 0.4554(7) 0.5873(3) 0.8026(7) 0.087(3) Uani 1 1 d . . . H6A H 0.4425 0.5813 0.8757 0.131 Uiso 1 1 calc R . . H6B H 0.5101 0.5950 0.7993 0.131 Uiso 1 1 calc R . . H6C H 0.4494 0.5688 0.7561 0.131 Uiso 1 1 calc R . . C13 C 0.2772(7) 0.5278(2) 0.8219(7) 0.079(3) Uani 1 1 d . . . H3A H 0.3342 0.5266 0.8076 0.118 Uiso 1 1 calc R . . H3B H 0.2480 0.5196 0.7606 0.118 Uiso 1 1 calc R . . H3C H 0.2647 0.5149 0.8846 0.118 Uiso 1 1 calc R . . C14 C 0.1447(5) 0.5632(2) 0.8659(6) 0.072(3) Uani 1 1 d . . . H4A H 0.1207 0.5833 0.8884 0.108 Uiso 1 1 calc R . . H4B H 0.1363 0.5471 0.9208 0.108 Uiso 1 1 calc R . . H4C H 0.1203 0.5562 0.7994 0.108 Uiso 1 1 calc R . . C15 C 0.2081(6) 0.6503(2) 0.9099(6) 0.078(3) Uani 1 1 d . . . H7A H 0.1864 0.6324 0.9502 0.117 Uiso 1 1 calc R . . H7B H 0.1786 0.6697 0.9271 0.117 Uiso 1 1 calc R . . H7C H 0.2640 0.6532 0.9285 0.117 Uiso 1 1 calc R . . C16 C 0.2328(7) 0.6798(2) 0.7211(7) 0.085(3) Uani 1 1 d . . . H8A H 0.2307 0.6801 0.6433 0.128 Uiso 1 1 calc R . . H8B H 0.2873 0.6835 0.7445 0.128 Uiso 1 1 calc R . . H8C H 0.1985 0.6967 0.7492 0.128 Uiso 1 1 calc R . . O3 O 0.3320(4) 0.56066(13) 0.6199(4) 0.0683(17) Uani 1 1 d . . . S8 S 0.32091(16) 0.53896(5) 0.52711(15) 0.0684(6) Uani 1 1 d D . . O10 O 0.3165(5) 0.50583(14) 0.5571(5) 0.105(3) Uani 1 1 d D . . O11 O 0.2623(4) 0.54945(17) 0.4498(4) 0.094(2) Uani 1 1 d D . . C17 C 0.4226(8) 0.5437(3) 0.4637(8) 0.097(4) Uani 1 1 d D . . F1 F 0.4231(5) 0.5225(2) 0.3784(6) 0.165(4) Uani 1 1 d D . . F2 F 0.4779(5) 0.5380(2) 0.5266(7) 0.150(3) Uani 1 1 d D . . F3 F 0.4237(6) 0.5744(2) 0.4254(6) 0.166(4) Uani 1 1 d . . . S20 S 0.3380(6) 0.7500 0.3250(6) 0.173(3) Uani 1 2 d SD . . O20 O 0.4189(13) 0.7500 0.271(2) 0.295(13) Uiso 1 2 d SD . . O21 O 0.3027(13) 0.7814(4) 0.2948(14) 0.317(10) Uiso 1 1 d D . . C20 C 0.3684(19) 0.7500 0.4727(18) 0.31(2) Uiso 1 2 d SD . . F20 F 0.2900(17) 0.7500 0.521(2) 0.377(15) Uiso 1 2 d SD . . F21 F 0.3858(10) 0.7789(4) 0.4936(14) 0.336(8) Uiso 1 1 d D . . S30 S 0.1547(4) 0.7500 -0.0308(3) 0.1118(17) Uani 1 2 d SD . . O30 O 0.1386(16) 0.7500 0.0858(13) 0.143(9) Uiso 0.50 2 d SPD . . O31 O 0.1262(10) 0.7787(3) -0.0844(12) 0.110(5) Uiso 0.50 1 d PD . . C30 C 0.2691(12) 0.7500 -0.021(2) 0.249(18) Uiso 1 2 d SD . . F30 F 0.2871(15) 0.7500 -0.1341(19) 0.179(10) Uiso 0.50 2 d SPD . . F31 F 0.2827(12) 0.7743(5) 0.0337(16) 0.166(7) Uiso 0.50 1 d PD . . O32 O 0.156(3) 0.7500 -0.170(3) 0.248(19) Uiso 0.50 2 d SP . . O33 O 0.1208(17) 0.7835(6) -0.016(2) 0.197(11) Uiso 0.50 1 d P . . F32 F 0.272(4) 0.7500 0.078(3) 0.34(3) Uiso 0.50 2 d SP . . F33 F 0.3027(12) 0.7752(5) -0.0383(15) 0.156(6) Uiso 0.50 1 d P . . C40 C 0.5191(11) 0.7500 0.774(2) 0.168(10) Uani 1 2 d S . . H40 H 0.5430 0.7500 0.7018 0.202 Uiso 1 2 calc SR . . Cl1 Cl 0.5950(9) 0.7500 0.8662(7) 0.288(6) Uani 1 2 d S . . Cl2 Cl 0.4722(5) 0.78482(14) 0.7921(5) 0.238(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0670(6) 0.0644(4) 0.0440(3) 0.0009(2) -0.0042(3) -0.0067(3) S1 0.068(2) 0.0878(15) 0.0576(10) 0.0000(9) -0.0041(10) 0.0047(12) S2 0.101(3) 0.0811(14) 0.0581(10) 0.0139(9) -0.0025(11) -0.0122(13) S3 0.130(3) 0.0711(13) 0.0585(11) -0.0102(9) -0.0022(13) -0.0006(14) C1 0.079(11) 0.129(9) 0.070(5) 0.025(5) -0.010(5) 0.010(7) C2 0.115(12) 0.135(9) 0.055(5) 0.018(5) -0.005(5) 0.035(8) C3 0.184(16) 0.078(7) 0.103(7) 0.017(5) -0.003(8) -0.017(8) C4 0.204(17) 0.076(6) 0.090(7) -0.009(5) 0.017(8) -0.029(8) C5 0.146(13) 0.084(7) 0.076(5) -0.002(5) 0.011(6) 0.039(7) C6 0.090(11) 0.120(8) 0.085(6) 0.003(6) 0.023(6) 0.021(7) S4 0.064(2) 0.0901(14) 0.0503(9) -0.0081(8) -0.0023(9) 0.0046(11) O4 0.086(6) 0.117(5) 0.053(3) -0.013(3) -0.013(3) 0.017(4) C7 0.092(13) 0.212(14) 0.058(5) -0.010(6) 0.002(5) 0.017(10) C8 0.133(12) 0.078(6) 0.094(6) -0.019(5) -0.010(6) 0.005(6) O1 0.060(5) 0.087(4) 0.049(2) 0.010(2) -0.006(2) -0.021(3) O2 0.059(5) 0.068(3) 0.046(2) 0.001(2) -0.006(2) 0.000(3) C9 0.062(7) 0.060(4) 0.045(3) 0.001(3) 0.002(4) -0.008(4) C10 0.074(8) 0.057(4) 0.046(3) -0.004(3) 0.002(4) 0.000(4) O8 0.070(5) 0.066(3) 0.044(2) -0.001(2) 0.000(2) -0.009(3) O9 0.053(5) 0.078(3) 0.049(2) 0.004(2) -0.004(2) -0.014(3) Ru2 0.0468(5) 0.0666(4) 0.0423(3) -0.0023(2) 0.0005(2) -0.0036(3) S5 0.0483(18) 0.0844(13) 0.0528(9) -0.0050(8) -0.0037(9) -0.0096(10) O5 0.063(6) 0.105(4) 0.073(3) -0.024(3) -0.007(3) -0.009(4) S6 0.056(2) 0.0791(13) 0.0477(9) 0.0037(8) 0.0013(8) 0.0004(10) O6 0.071(6) 0.109(4) 0.046(2) 0.002(2) -0.010(3) 0.001(3) S7 0.057(2) 0.0727(12) 0.0611(10) -0.0085(8) 0.0027(10) 0.0001(10) O7 0.041(6) 0.104(5) 0.112(5) -0.029(4) -0.007(4) 0.007(3) C11 0.048(8) 0.136(8) 0.068(5) 0.006(5) -0.007(5) -0.024(6) C12 0.068(10) 0.110(7) 0.084(5) 0.000(5) -0.007(5) 0.010(6) C13 0.068(9) 0.073(5) 0.095(6) 0.010(4) 0.003(5) 0.008(5) C14 0.041(7) 0.117(7) 0.059(4) -0.001(4) 0.011(4) -0.019(5) C15 0.079(9) 0.098(6) 0.057(4) -0.009(4) 0.008(4) 0.001(5) C16 0.101(10) 0.067(5) 0.088(6) -0.001(4) 0.003(6) -0.003(5) O3 0.076(5) 0.079(3) 0.049(2) -0.009(2) 0.002(3) 0.006(3) S8 0.071(2) 0.0775(13) 0.0565(10) -0.0100(8) 0.0010(10) 0.0022(11) O10 0.147(8) 0.071(4) 0.097(4) 0.003(3) 0.004(4) -0.019(4) O11 0.076(6) 0.128(5) 0.077(4) -0.030(3) -0.017(3) 0.030(4) C17 0.098(13) 0.115(9) 0.077(6) -0.022(6) 0.024(6) -0.004(7) F1 0.148(9) 0.214(8) 0.132(5) -0.077(6) 0.078(5) -0.018(7) F2 0.064(7) 0.239(9) 0.145(6) -0.053(6) -0.012(5) 0.036(6) F3 0.188(11) 0.165(7) 0.144(6) -0.001(5) 0.070(6) -0.062(7) S20 0.185(9) 0.109(4) 0.226(7) 0.000 -0.006(6) 0.000 S30 0.165(6) 0.078(2) 0.093(2) 0.000 0.023(3) 0.000 C40 0.20(3) 0.090(13) 0.21(2) 0.000 -0.04(2) 0.000 Cl1 0.50(2) 0.204(8) 0.162(6) 0.000 -0.094(9) 0.000 Cl2 0.323(10) 0.171(5) 0.220(5) -0.020(4) 0.010(5) 0.073(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 O1 2.131(6) . ? Ru1 O2 2.176(4) . ? Ru1 S4 2.276(2) . ? Ru1 S1 2.281(3) . ? Ru1 S2 2.282(2) . ? Ru1 S3 2.338(2) . ? S1 C6 1.820(10) . ? S1 C1 1.877(9) . ? S2 C2 1.807(11) . ? S2 C3 1.847(11) . ? S3 C5 1.784(13) . ? S3 C4 1.824(10) . ? C1 C2 1.501(14) . ? C3 C4 1.489(14) . ? C5 C6 1.571(15) . ? S4 O4 1.475(5) . ? S4 C7 1.739(12) . ? S4 C8 1.783(10) . ? O1 C9 1.261(8) . ? O2 C10 1.247(10) . ? C9 O9 1.246(9) . ? C9 C10 1.538(11) . ? C10 O8 1.278(8) . ? O8 Ru2 2.127(5) . ? O9 Ru2 2.123(4) . ? Ru2 O3 2.164(5) . ? Ru2 S6 2.2425(19) . ? Ru2 S5 2.247(2) . ? Ru2 S7 2.247(2) . ? S5 O5 1.464(6) . ? S5 C12 1.791(10) . ? S5 C11 1.804(9) . ? S6 O6 1.474(5) . ? S6 C14 1.765(9) . ? S6 C13 1.779(9) . ? S7 O7 1.472(7) . ? S7 C16 1.748(9) . ? S7 C15 1.779(7) . ? O3 S8 1.464(5) . ? S8 O10 1.415(6) . ? S8 O11 1.428(6) . ? S8 C17 1.866(12) . ? C17 F2 1.223(12) . ? C17 F3 1.351(13) . ? C17 F1 1.368(11) . ? S20 O21 1.468(14) 8_575 ? S20 O21 1.468(14) . ? S20 O20 1.494(17) . ? S20 C20 1.89(2) . ? C20 F21 1.251(15) . ? C20 F21 1.251(15) 8_575 ? C20 F20 1.43(2) . ? S30 O31 1.433(12) 8_575 ? S30 O31 1.433(12) . ? S30 O30 1.464(15) . ? S30 O33 1.50(3) 8_575 ? S30 O33 1.50(3) . ? S30 O32 1.72(3) . ? S30 C30 1.90(2) . ? O31 O33 0.87(2) . ? O31 O32 1.66(2) . ? C30 F33 1.19(2) . ? C30 F33 1.19(2) 8_575 ? C30 F32 1.22(3) . ? C30 F31 1.230(16) . ? C30 F31 1.230(16) 8_575 ? C30 F30 1.423(19) . ? F30 F33 1.59(3) . ? F30 F33 1.59(3) 8_575 ? F31 F33 0.95(2) . ? F31 F32 1.15(3) . ? O32 O31 1.66(2) 8_575 ? F32 F31 1.15(3) 8_575 ? C40 Cl2 1.645(11) . ? C40 Cl2 1.645(11) 8_575 ? C40 Cl1 1.692(15) . ? 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 O1 Ru1 O2 78.3(2) . . ? O1 Ru1 S4 93.12(17) . . ? O2 Ru1 S4 93.47(14) . . ? O1 Ru1 S1 173.67(15) . . ? O2 Ru1 S1 98.42(17) . . ? S4 Ru1 S1 92.48(9) . . ? O1 Ru1 S2 94.98(15) . . ? O2 Ru1 S2 172.88(16) . . ? S4 Ru1 S2 89.21(9) . . ? S1 Ru1 S2 88.04(9) . . ? O1 Ru1 S3 86.53(17) . . ? O2 Ru1 S3 88.05(14) . . ? S4 Ru1 S3 178.34(9) . . ? S1 Ru1 S3 87.96(10) . . ? S2 Ru1 S3 89.20(9) . . ? C6 S1 C1 99.4(5) . . ? C6 S1 Ru1 105.7(4) . . ? C1 S1 Ru1 107.5(4) . . ? C2 S2 C3 100.0(6) . . ? C2 S2 Ru1 105.3(4) . . ? C3 S2 Ru1 105.6(3) . . ? C5 S3 C4 102.4(6) . . ? C5 S3 Ru1 106.0(3) . . ? C4 S3 Ru1 100.8(4) . . ? C2 C1 S1 110.7(7) . . ? C1 C2 S2 116.1(6) . . ? C4 C3 S2 112.7(7) . . ? C3 C4 S3 115.2(8) . . ? C6 C5 S3 114.4(7) . . ? C5 C6 S1 111.4(8) . . ? O4 S4 C7 108.1(4) . . ? O4 S4 C8 107.1(5) . . ? C7 S4 C8 99.9(7) . . ? O4 S4 Ru1 116.3(3) . . ? C7 S4 Ru1 113.3(4) . . ? C8 S4 Ru1 110.7(3) . . ? C9 O1 Ru1 112.4(5) . . ? C10 O2 Ru1 110.8(5) . . ? O9 C9 O1 123.7(7) . . ? O9 C9 C10 119.2(6) . . ? O1 C9 C10 117.1(7) . . ? O2 C10 O8 124.9(8) . . ? O2 C10 C9 119.0(6) . . ? O8 C10 C9 116.0(7) . . ? C10 O8 Ru2 112.9(5) . . ? C9 O9 Ru2 112.5(5) . . ? O9 Ru2 O8 79.15(19) . . ? O9 Ru2 O3 86.1(2) . . ? O8 Ru2 O3 87.6(2) . . ? O9 Ru2 S6 172.79(15) . . ? O8 Ru2 S6 94.47(14) . . ? O3 Ru2 S6 90.30(14) . . ? O9 Ru2 S5 92.65(16) . . ? O8 Ru2 S5 171.28(13) . . ? O3 Ru2 S5 88.94(18) . . ? S6 Ru2 S5 93.54(8) . . ? O9 Ru2 S7 89.90(16) . . ? O8 Ru2 S7 89.55(16) . . ? O3 Ru2 S7 175.45(14) . . ? S6 Ru2 S7 93.43(8) . . ? S5 Ru2 S7 93.41(9) . . ? O5 S5 C12 106.8(4) . . ? O5 S5 C11 106.9(4) . . ? C12 S5 C11 101.7(5) . . ? O5 S5 Ru2 119.4(3) . . ? C12 S5 Ru2 113.2(4) . . ? C11 S5 Ru2 107.3(3) . . ? O6 S6 C14 108.6(4) . . ? O6 S6 C13 107.4(4) . . ? C14 S6 C13 98.8(5) . . ? O6 S6 Ru2 118.8(3) . . ? C14 S6 Ru2 109.4(3) . . ? C13 S6 Ru2 111.9(3) . . ? O7 S7 C16 105.8(5) . . ? O7 S7 C15 107.2(4) . . ? C16 S7 C15 97.9(4) . . ? O7 S7 Ru2 112.4(3) . . ? C16 S7 Ru2 113.4(4) . . ? C15 S7 Ru2 118.6(3) . . ? S8 O3 Ru2 138.7(4) . . ? O10 S8 O11 115.5(5) . . ? O10 S8 O3 113.0(4) . . ? O11 S8 O3 115.0(4) . . ? O10 S8 C17 104.9(5) . . ? O11 S8 C17 107.5(5) . . ? O3 S8 C17 98.7(4) . . ? F2 C17 F3 113.2(12) . . ? F2 C17 F1 111.1(11) . . ? F3 C17 F1 109.2(9) . . ? F2 C17 S8 112.9(8) . . ? F3 C17 S8 104.9(9) . . ? F1 C17 S8 105.1(8) . . ? O21 S20 O21 123.6(18) 8_575 . ? O21 S20 O20 104.2(10) 8_575 . ? O21 S20 O20 104.2(10) . . ? O21 S20 C20 110.5(9) 8_575 . ? O21 S20 C20 110.5(9) . . ? O20 S20 C20 100.9(14) . . ? F21 C20 F21 144(3) . 8_575 ? F21 C20 F20 97.0(17) . . ? F21 C20 F20 97.0(17) 8_575 . ? F21 C20 S20 105.1(14) . . ? F21 C20 S20 105.1(14) 8_575 . ? F20 C20 S20 99.4(18) . . ? O31 S30 O31 111.0(14) 8_575 . ? O31 S30 O30 113.2(8) 8_575 . ? O31 S30 O30 113.2(8) . . ? O31 S30 O33 34.4(10) 8_575 8_575 ? O31 S30 O33 133.7(13) . 8_575 ? O30 S30 O33 79.2(11) . 8_575 ? O31 S30 O33 133.7(13) 8_575 . ? O31 S30 O33 34.4(10) . . ? O30 S30 O33 79.2(11) . . ? O33 S30 O33 134(2) 8_575 . ? O31 S30 O32 62.7(9) 8_575 . ? O31 S30 O32 62.7(9) . . ? O30 S30 O32 170(2) . . ? O33 S30 O32 97.2(12) 8_575 . ? O33 S30 O32 97.2(12) . . ? O31 S30 C30 110.9(8) 8_575 . ? O31 S30 C30 110.9(8) . . ? O30 S30 C30 96.9(12) . . ? O33 S30 C30 111.4(11) 8_575 . ? O33 S30 C30 111.4(11) . . ? O32 S30 C30 93.0(19) . . ? O33 O31 S30 77(2) . . ? O33 O31 O32 144(2) . . ? S30 O31 O32 67.0(13) . . ? F33 C30 F33 120(3) . 8_575 ? F33 C30 F32 99(2) . . ? F33 C30 F32 99(2) 8_575 . ? F33 C30 F31 46.1(11) . . ? F33 C30 F31 136(2) 8_575 . ? F32 C30 F31 56.0(16) . . ? F33 C30 F31 136(2) . 8_575 ? F33 C30 F31 46.1(11) 8_575 8_575 ? F32 C30 F31 56.0(16) . 8_575 ? F31 C30 F31 109(3) . 8_575 ? F33 C30 F30 74.4(16) . . ? F33 C30 F30 74.4(16) 8_575 . ? F32 C30 F30 166(4) . . ? F31 C30 F30 120.1(16) . . ? F31 C30 F30 120.1(16) 8_575 . ? F33 C30 S30 117.0(14) . . ? F33 C30 S30 117.0(14) 8_575 . ? F32 C30 S30 96(3) . . ? F31 C30 S30 102.5(15) . . ? F31 C30 S30 102.5(15) 8_575 . ? F30 C30 S30 98.5(17) . . ? C30 F30 F33 46.2(9) . . ? C30 F30 F33 46.2(9) . 8_575 ? F33 F30 F33 81.2(16) . 8_575 ? F33 F31 F32 122(3) . . ? F33 F31 C30 65.0(15) . . ? F32 F31 C30 61.6(16) . . ? O31 O32 O31 90.9(18) 8_575 . ? O31 O32 S30 50.3(9) 8_575 . ? O31 O32 S30 50.3(9) . . ? O31 O33 S30 68.5(18) . . ? F31 F32 F31 121(4) . 8_575 ? F31 F32 C30 62.3(16) . . ? F31 F32 C30 62.3(16) 8_575 . ? F31 F33 C30 68.9(17) . . ? F31 F33 F30 128(2) . . ? C30 F33 F30 59.3(14) . . ? Cl2 C40 Cl2 121.3(15) . 8_575 ? Cl2 C40 Cl1 105.2(10) . . ? Cl2 C40 Cl1 105.2(10) 8_575 . ? 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 O1 Ru1 S1 C6 11.8(15) . . . . ? O2 Ru1 S1 C6 70.1(4) . . . . ? S4 Ru1 S1 C6 163.9(4) . . . . ? S2 Ru1 S1 C6 -106.9(4) . . . . ? S3 Ru1 S1 C6 -17.7(4) . . . . ? O1 Ru1 S1 C1 117.2(14) . . . . ? O2 Ru1 S1 C1 175.6(4) . . . . ? S4 Ru1 S1 C1 -90.6(4) . . . . ? S2 Ru1 S1 C1 -1.4(4) . . . . ? S3 Ru1 S1 C1 87.8(4) . . . . ? O1 Ru1 S2 C2 169.8(4) . . . . ? O2 Ru1 S2 C2 -171.0(13) . . . . ? S4 Ru1 S2 C2 76.7(4) . . . . ? S1 Ru1 S2 C2 -15.8(4) . . . . ? S3 Ru1 S2 C2 -103.8(4) . . . . ? O1 Ru1 S2 C3 -84.9(5) . . . . ? O2 Ru1 S2 C3 -65.7(14) . . . . ? S4 Ru1 S2 C3 -178.0(5) . . . . ? S1 Ru1 S2 C3 89.5(5) . . . . ? S3 Ru1 S2 C3 1.5(5) . . . . ? O1 Ru1 S3 C5 -178.8(4) . . . . ? O2 Ru1 S3 C5 -100.4(4) . . . . ? S4 Ru1 S3 C5 104(4) . . . . ? S1 Ru1 S3 C5 -1.9(4) . . . . ? S2 Ru1 S3 C5 86.2(4) . . . . ? O1 Ru1 S3 C4 74.9(5) . . . . ? O2 Ru1 S3 C4 153.3(5) . . . . ? S4 Ru1 S3 C4 -3(4) . . . . ? S1 Ru1 S3 C4 -108.2(5) . . . . ? S2 Ru1 S3 C4 -20.2(5) . . . . ? C6 S1 C1 C2 132.6(8) . . . . ? Ru1 S1 C1 C2 22.7(9) . . . . ? S1 C1 C2 S2 -39.1(11) . . . . ? C3 S2 C2 C1 -73.0(9) . . . . ? Ru1 S2 C2 C1 36.4(9) . . . . ? C2 S2 C3 C4 132.5(10) . . . . ? Ru1 S2 C3 C4 23.4(11) . . . . ? S2 C3 C4 S3 -45.0(14) . . . . ? C5 S3 C4 C3 -67.0(11) . . . . ? Ru1 S3 C4 C3 42.1(11) . . . . ? C4 S3 C5 C6 130.9(7) . . . . ? Ru1 S3 C5 C6 25.7(7) . . . . ? S3 C5 C6 S1 -42.5(9) . . . . ? C1 S1 C6 C5 -73.7(8) . . . . ? Ru1 S1 C6 C5 37.6(8) . . . . ? O1 Ru1 S4 O4 -136.0(4) . . . . ? O2 Ru1 S4 O4 145.5(4) . . . . ? S1 Ru1 S4 O4 46.9(4) . . . . ? S2 Ru1 S4 O4 -41.1(4) . . . . ? S3 Ru1 S4 O4 -58(4) . . . . ? O1 Ru1 S4 C7 -9.9(5) . . . . ? O2 Ru1 S4 C7 -88.4(5) . . . . ? S1 Ru1 S4 C7 173.0(5) . . . . ? S2 Ru1 S4 C7 85.0(5) . . . . ? S3 Ru1 S4 C7 68(4) . . . . ? O1 Ru1 S4 C8 101.4(5) . . . . ? O2 Ru1 S4 C8 22.9(5) . . . . ? S1 Ru1 S4 C8 -75.7(4) . . . . ? S2 Ru1 S4 C8 -163.7(4) . . . . ? S3 Ru1 S4 C8 179(100) . . . . ? O2 Ru1 O1 C9 -13.6(5) . . . . ? S4 Ru1 O1 C9 -106.5(5) . . . . ? S1 Ru1 O1 C9 45.7(17) . . . . ? S2 Ru1 O1 C9 164.1(5) . . . . ? S3 Ru1 O1 C9 75.2(5) . . . . ? O1 Ru1 O2 C10 11.6(5) . . . . ? S4 Ru1 O2 C10 104.1(5) . . . . ? S1 Ru1 O2 C10 -162.9(5) . . . . ? S2 Ru1 O2 C10 -7.9(16) . . . . ? S3 Ru1 O2 C10 -75.2(5) . . . . ? Ru1 O1 C9 O9 -167.6(6) . . . . ? Ru1 O1 C9 C10 13.5(8) . . . . ? Ru1 O2 C10 O8 173.3(6) . . . . ? Ru1 O2 C10 C9 -8.6(8) . . . . ? O9 C9 C10 O2 177.8(7) . . . . ? O1 C9 C10 O2 -3.2(11) . . . . ? O9 C9 C10 O8 -4.0(10) . . . . ? O1 C9 C10 O8 175.0(7) . . . . ? O2 C10 O8 Ru2 -175.6(6) . . . . ? C9 C10 O8 Ru2 6.3(8) . . . . ? O1 C9 O9 Ru2 -179.6(6) . . . . ? C10 C9 O9 Ru2 -0.7(9) . . . . ? C9 O9 Ru2 O8 3.0(5) . . . . ? C9 O9 Ru2 O3 91.2(5) . . . . ? C9 O9 Ru2 S6 31.0(18) . . . . ? C9 O9 Ru2 S5 180.0(5) . . . . ? C9 O9 Ru2 S7 -86.6(5) . . . . ? C10 O8 Ru2 O9 -5.2(5) . . . . ? C10 O8 Ru2 O3 -91.7(5) . . . . ? C10 O8 Ru2 S6 178.2(5) . . . . ? C10 O8 Ru2 S5 -25.1(13) . . . . ? C10 O8 Ru2 S7 84.8(5) . . . . ? O9 Ru2 S5 O5 106.5(4) . . . . ? O8 Ru2 S5 O5 126.1(10) . . . . ? O3 Ru2 S5 O5 -167.5(4) . . . . ? S6 Ru2 S5 O5 -77.3(3) . . . . ? S7 Ru2 S5 O5 16.4(3) . . . . ? O9 Ru2 S5 C12 -126.6(4) . . . . ? O8 Ru2 S5 C12 -106.9(11) . . . . ? O3 Ru2 S5 C12 -40.5(4) . . . . ? S6 Ru2 S5 C12 49.7(3) . . . . ? S7 Ru2 S5 C12 143.4(3) . . . . ? O9 Ru2 S5 C11 -15.2(4) . . . . ? O8 Ru2 S5 C11 4.4(11) . . . . ? O3 Ru2 S5 C11 70.8(4) . . . . ? S6 Ru2 S5 C11 161.0(4) . . . . ? S7 Ru2 S5 C11 -105.3(4) . . . . ? O9 Ru2 S6 O6 177.1(14) . . . . ? O8 Ru2 S6 O6 -155.3(3) . . . . ? O3 Ru2 S6 O6 117.1(4) . . . . ? S5 Ru2 S6 O6 28.1(3) . . . . ? S7 Ru2 S6 O6 -65.5(3) . . . . ? O9 Ru2 S6 C14 -57.5(15) . . . . ? O8 Ru2 S6 C14 -29.9(4) . . . . ? O3 Ru2 S6 C14 -117.5(4) . . . . ? S5 Ru2 S6 C14 153.5(3) . . . . ? S7 Ru2 S6 C14 59.9(3) . . . . ? O9 Ru2 S6 C13 51.0(15) . . . . ? O8 Ru2 S6 C13 78.5(4) . . . . ? O3 Ru2 S6 C13 -9.1(4) . . . . ? S5 Ru2 S6 C13 -98.0(4) . . . . ? S7 Ru2 S6 C13 168.4(4) . . . . ? O9 Ru2 S7 O7 84.7(4) . . . . ? O8 Ru2 S7 O7 5.5(4) . . . . ? O3 Ru2 S7 O7 56(2) . . . . ? S6 Ru2 S7 O7 -88.9(3) . . . . ? S5 Ru2 S7 O7 177.3(3) . . . . ? O9 Ru2 S7 C16 -35.3(4) . . . . ? O8 Ru2 S7 C16 -114.4(4) . . . . ? O3 Ru2 S7 C16 -64(2) . . . . ? S6 Ru2 S7 C16 151.1(4) . . . . ? S5 Ru2 S7 C16 57.3(4) . . . . ? O9 Ru2 S7 C15 -149.3(4) . . . . ? O8 Ru2 S7 C15 131.6(4) . . . . ? O3 Ru2 S7 C15 -178(21) . . . . ? S6 Ru2 S7 C15 37.1(4) . . . . ? S5 Ru2 S7 C15 -56.6(4) . . . . ? O9 Ru2 O3 S8 -60.7(5) . . . . ? O8 Ru2 O3 S8 18.6(5) . . . . ? S6 Ru2 O3 S8 113.1(5) . . . . ? S5 Ru2 O3 S8 -153.4(5) . . . . ? S7 Ru2 O3 S8 -32(3) . . . . ? Ru2 O3 S8 O10 -118.1(6) . . . . ? Ru2 O3 S8 O11 17.5(7) . . . . ? Ru2 O3 S8 C17 131.5(6) . . . . ? O10 S8 C17 F2 -62.3(10) . . . . ? O11 S8 C17 F2 174.2(8) . . . . ? O3 S8 C17 F2 54.4(9) . . . . ? O10 S8 C17 F3 174.0(7) . . . . ? O11 S8 C17 F3 50.5(8) . . . . ? O3 S8 C17 F3 -69.3(8) . . . . ? O10 S8 C17 F1 58.9(9) . . . . ? O11 S8 C17 F1 -64.6(9) . . . . ? O3 S8 C17 F1 175.6(8) . . . . ? O21 S20 C20 F21 -170(2) 8_575 . . . ? O21 S20 C20 F21 -30(3) . . . . ? O20 S20 C20 F21 80(2) . . . . ? O21 S20 C20 F21 30(3) 8_575 . . 8_575 ? O21 S20 C20 F21 170(2) . . . 8_575 ? O20 S20 C20 F21 -80(2) . . . 8_575 ? O21 S20 C20 F20 -70.3(11) 8_575 . . . ? O21 S20 C20 F20 70.3(11) . . . . ? O20 S20 C20 F20 180.000(2) . . . . ? O31 S30 O31 O33 139(2) 8_575 . . . ? O30 S30 O31 O33 10(3) . . . . ? O33 S30 O31 O33 107(3) 8_575 . . . ? O32 S30 O31 O33 -180(3) . . . . ? C30 S30 O31 O33 -98(2) . . . . ? O31 S30 O31 O32 -41(2) 8_575 . . . ? O30 S30 O31 O32 -170(2) . . . . ? O33 S30 O31 O32 -73(2) 8_575 . . . ? O33 S30 O31 O32 180(3) . . . . ? C30 S30 O31 O32 82(2) . . . . ? O31 S30 C30 F33 139(2) 8_575 . . . ? O31 S30 C30 F33 15(2) . . . . ? O30 S30 C30 F33 -103(2) . . . . ? O33 S30 C30 F33 176(2) 8_575 . . . ? O33 S30 C30 F33 -22(3) . . . . ? O32 S30 C30 F33 77(2) . . . . ? O31 S30 C30 F33 -15(2) 8_575 . . 8_575 ? O31 S30 C30 F33 -139(2) . . . 8_575 ? O30 S30 C30 F33 103(2) . . . 8_575 ? O33 S30 C30 F33 22(3) 8_575 . . 8_575 ? O33 S30 C30 F33 -176(2) . . . 8_575 ? O32 S30 C30 F33 -77(2) . . . 8_575 ? O31 S30 C30 F32 -118.1(8) 8_575 . . . ? O31 S30 C30 F32 118.1(8) . . . . ? O30 S30 C30 F32 0.000(2) . . . . ? O33 S30 C30 F32 -81.1(12) 8_575 . . . ? O33 S30 C30 F32 81.1(12) . . . . ? O32 S30 C30 F32 180.000(2) . . . . ? O31 S30 C30 F31 -174.5(16) 8_575 . . . ? O31 S30 C30 F31 62(2) . . . . ? O30 S30 C30 F31 -56.4(16) . . . . ? O33 S30 C30 F31 -137.5(18) 8_575 . . . ? O33 S30 C30 F31 25(2) . . . . ? O32 S30 C30 F31 123.6(16) . . . . ? O31 S30 C30 F31 -62(2) 8_575 . . 8_575 ? O31 S30 C30 F31 174.5(16) . . . 8_575 ? O30 S30 C30 F31 56.4(16) . . . 8_575 ? O33 S30 C30 F31 -25(2) 8_575 . . 8_575 ? O33 S30 C30 F31 137.5(18) . . . 8_575 ? O32 S30 C30 F31 -123.6(16) . . . 8_575 ? O31 S30 C30 F30 61.9(8) 8_575 . . . ? O31 S30 C30 F30 -61.9(8) . . . . ? O30 S30 C30 F30 180.000(4) . . . . ? O33 S30 C30 F30 98.9(12) 8_575 . . . ? O33 S30 C30 F30 -98.9(12) . . . . ? O32 S30 C30 F30 0.0 . . . . ? F33 C30 F30 F33 -129(3) 8_575 . . . ? F32 C30 F30 F33 -64.3(13) . . . . ? F31 C30 F30 F33 6(2) . . . . ? F31 C30 F30 F33 -134(3) 8_575 . . . ? S30 C30 F30 F33 115.7(13) . . . . ? F33 C30 F30 F33 129(3) . . . 8_575 ? F32 C30 F30 F33 64.3(13) . . . 8_575 ? F31 C30 F30 F33 134(3) . . . 8_575 ? F31 C30 F30 F33 -6(2) 8_575 . . 8_575 ? S30 C30 F30 F33 -115.7(13) . . . 8_575 ? F33 C30 F31 F33 91(4) 8_575 . . . ? F32 C30 F31 F33 156(5) . . . . ? F31 C30 F31 F33 136(2) 8_575 . . . ? F30 C30 F31 F33 -8(3) . . . . ? S30 C30 F31 F33 -116(2) . . . . ? F33 C30 F31 F32 -156(5) . . . . ? F33 C30 F31 F32 -65(5) 8_575 . . . ? F31 C30 F31 F32 -20(5) 8_575 . . . ? F30 C30 F31 F32 -164(4) . . . . ? S30 C30 F31 F32 88(4) . . . . ? O33 O31 O32 O31 32(7) . . . 8_575 ? S30 O31 O32 O31 32.4(16) . . . 8_575 ? O33 O31 O32 S30 0(6) . . . . ? O31 S30 O32 O31 -136(2) . . . 8_575 ? O30 S30 O32 O31 -67.9(12) . . . 8_575 ? O33 S30 O32 O31 0.0(19) 8_575 . . 8_575 ? O33 S30 O32 O31 -135.9(14) . . . 8_575 ? C30 S30 O32 O31 112.1(12) . . . 8_575 ? O31 S30 O32 O31 136(2) 8_575 . . . ? O30 S30 O32 O31 67.9(12) . . . . ? O33 S30 O32 O31 135.9(14) 8_575 . . . ? O33 S30 O32 O31 0.0(19) . . . . ? C30 S30 O32 O31 -112.1(12) . . . . ? O32 O31 O33 S30 0(5) . . . . ? O31 S30 O33 O31 -59(3) 8_575 . . . ? O30 S30 O33 O31 -171(3) . . . . ? O33 S30 O33 O31 -107(3) 8_575 . . . ? O32 S30 O33 O31 0(3) . . . . ? C30 S30 O33 O31 96(2) . . . . ? F33 F31 F32 F31 -2(9) . . . 8_575 ? C30 F31 F32 F31 23(5) . . . 8_575 ? F33 F31 F32 C30 -26(5) . . . . ? F33 C30 F32 F31 17(3) . . . . ? F33 C30 F32 F31 140(3) 8_575 . . . ? F31 C30 F32 F31 157(5) 8_575 . . . ? F30 C30 F32 F31 79(3) . . . . ? S30 C30 F32 F31 -101(3) . . . . ? F33 C30 F32 F31 -140(3) . . . 8_575 ? F33 C30 F32 F31 -17(3) 8_575 . . 8_575 ? F31 C30 F32 F31 -157(5) . . . 8_575 ? F30 C30 F32 F31 -79(3) . . . 8_575 ? S30 C30 F32 F31 101(3) . . . 8_575 ? F32 F31 F33 C30 25(5) . . . . ? F32 F31 F33 F30 33(6) . . . . ? C30 F31 F33 F30 8(3) . . . . ? F33 C30 F33 F31 -126(3) 8_575 . . . ? F32 C30 F33 F31 -20(4) . . . . ? F31 C30 F33 F31 -70(4) 8_575 . . . ? F30 C30 F33 F31 173(3) . . . . ? S30 C30 F33 F31 81(2) . . . . ? F33 C30 F33 F30 61(3) 8_575 . . . ? F32 C30 F33 F30 167(3) . . . . ? F31 C30 F33 F30 -173(3) . . . . ? F31 C30 F33 F30 117(4) 8_575 . . . ? S30 C30 F33 F30 -92(2) . . . . ? C30 F30 F33 F31 -8(3) . . . . ? F33 F30 F33 F31 -43(4) 8_575 . . . ? F33 F30 F33 C30 -34.9(18) 8_575 . . . ? _diffrn_measured_fraction_theta_max 0.836 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.836 _refine_diff_density_max 1.055 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.120 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 646394' _audit_creation_method SHELXL-97 _chemical_name_systematic ; fac-(1,4,7-tritiacyclononane)-(dimethylsulfoxide,S)-ruthenium(II)-(mu-oxalate)- fac-tris(dimethylsulfoxide,S)-(dimethylsulfoxide,O)-ruthenium(II) bis(triflate) bis(nitromethane) solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H42 O9 Ru2 S8 2+, 2(C F3 S O3 1-), 2(C H3 N O2)' _chemical_formula_sum 'C22 H48 F6 N2 O19 Ru2 S10' _chemical_formula_weight 1281.36 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 15.284(3) _cell_length_b 16.305(3) _cell_length_c 19.628(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.22(2) _cell_angle_gamma 90.00 _cell_volume 4890.3(17) _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 yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.4579 _exptl_absorpt_correction_T_max 0.8254 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82752 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.28 _reflns_number_total 12046 _reflns_number_gt 8716 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (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^)+(0.1530P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12046 _refine_ls_number_parameters 510 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.2053 _refine_ls_wR_factor_gt 0.1954 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 1.059 _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 0.58766(2) 0.15545(2) 0.637256(18) 0.05070(14) Uani 1 1 d . . . S1 S 0.56378(8) 0.10584(8) 0.52972(6) 0.0610(3) Uani 1 1 d . . . S2 S 0.72554(8) 0.10260(9) 0.63388(7) 0.0622(3) Uani 1 1 d . . . S3 S 0.64026(9) 0.27557(8) 0.58893(7) 0.0638(3) Uani 1 1 d . . . S4 S 0.52759(8) 0.04765(8) 0.69631(7) 0.0620(3) Uani 1 1 d . . . O4 O 0.4500(3) 0.0709(3) 0.7356(2) 0.0902(13) Uani 1 1 d . . . C1 C 0.6648(4) 0.0553(5) 0.5055(3) 0.0869(19) Uani 1 1 d . . . H1A H 0.6498 0.0066 0.4793 0.104 Uiso 1 1 calc R . . H1B H 0.6966 0.0918 0.4759 0.104 Uiso 1 1 calc R . . C2 C 0.7226(4) 0.0313(5) 0.5621(4) 0.090(2) Uani 1 1 d . . . H2A H 0.7815 0.0255 0.5453 0.108 Uiso 1 1 calc R . . H2B H 0.7043 -0.0220 0.5785 0.108 Uiso 1 1 calc R . . C3 C 0.7946(4) 0.1820(5) 0.5972(4) 0.0857(18) Uani 1 1 d . . . H3A H 0.8514 0.1810 0.6202 0.103 Uiso 1 1 calc R . . H3B H 0.8034 0.1694 0.5495 0.103 Uiso 1 1 calc R . . C4 C 0.7573(4) 0.2659(4) 0.6025(4) 0.0883(19) Uani 1 1 d . . . H4A H 0.7859 0.3007 0.5696 0.106 Uiso 1 1 calc R . . H4B H 0.7719 0.2872 0.6474 0.106 Uiso 1 1 calc R . . C5 C 0.6314(5) 0.2605(5) 0.4961(3) 0.0910(19) Uani 1 1 d . . . H5A H 0.6155 0.3121 0.4746 0.109 Uiso 1 1 calc R . . H5B H 0.6880 0.2443 0.4792 0.109 Uiso 1 1 calc R . . C6 C 0.5658(5) 0.1976(4) 0.4765(3) 0.0801(16) Uani 1 1 d . . . H6A H 0.5765 0.1809 0.4300 0.096 Uiso 1 1 calc R . . H6B H 0.5083 0.2227 0.4770 0.096 Uiso 1 1 calc R . . C7 C 0.6038(5) 0.0042(5) 0.7550(4) 0.095(2) Uani 1 1 d . . . H7A H 0.6160 0.0425 0.7910 0.143 Uiso 1 1 calc R . . H7B H 0.6570 -0.0085 0.7320 0.143 Uiso 1 1 calc R . . H7C H 0.5798 -0.0451 0.7737 0.143 Uiso 1 1 calc R . . C8 C 0.4992(5) -0.0393(4) 0.6468(4) 0.092(2) Uani 1 1 d . . . H8A H 0.4581 -0.0236 0.6115 0.138 Uiso 1 1 calc R . . H8B H 0.4733 -0.0800 0.6754 0.138 Uiso 1 1 calc R . . H8C H 0.5509 -0.0614 0.6267 0.138 Uiso 1 1 calc R . . O1 O 0.6032(2) 0.2113(2) 0.73492(17) 0.0575(8) Uani 1 1 d . . . O2 O 0.4644(2) 0.2156(2) 0.64607(16) 0.0582(8) Uani 1 1 d . . . C9 C 0.5371(3) 0.2526(3) 0.7514(2) 0.0550(10) Uani 1 1 d . . . C10 C 0.4571(3) 0.2526(3) 0.7013(2) 0.0520(10) Uani 1 1 d . . . O8 O 0.3894(2) 0.2891(2) 0.72041(16) 0.0572(8) Uani 1 1 d . . . O9 O 0.5319(2) 0.2952(2) 0.80404(17) 0.0605(8) Uani 1 1 d . . . Ru2 Ru 0.41050(2) 0.35627(2) 0.812816(19) 0.05313(14) Uani 1 1 d . . . S5 S 0.45559(8) 0.42355(9) 0.90715(6) 0.0617(3) Uani 1 1 d . . . O5 O 0.3928(3) 0.4643(3) 0.9522(2) 0.0785(11) Uani 1 1 d . . . S6 S 0.28064(8) 0.42251(9) 0.80772(7) 0.0654(3) Uani 1 1 d . . . O6 O 0.2102(3) 0.3958(3) 0.8539(2) 0.0918(14) Uani 1 1 d . . . S7 S 0.35442(9) 0.25403(9) 0.87490(7) 0.0664(3) Uani 1 1 d . . . O7 O 0.3307(3) 0.2717(3) 0.9460(2) 0.0809(12) Uani 1 1 d . . . S8 S 0.51844(11) 0.44033(11) 0.68917(8) 0.0794(4) Uani 1 1 d . . . O3 O 0.4603(2) 0.4530(2) 0.75097(19) 0.0675(9) Uani 1 1 d . . . C11 C 0.5213(4) 0.3573(5) 0.9602(3) 0.0848(19) Uani 1 1 d . . . H11A H 0.4841 0.3194 0.9834 0.127 Uiso 1 1 calc R . . H11B H 0.5535 0.3895 0.9930 0.127 Uiso 1 1 calc R . . H11C H 0.5613 0.3274 0.9325 0.127 Uiso 1 1 calc R . . C12 C 0.5371(4) 0.4957(5) 0.8849(3) 0.088(2) Uani 1 1 d . . . H12A H 0.5210 0.5211 0.8423 0.132 Uiso 1 1 calc R . . H12B H 0.5922 0.4681 0.8805 0.132 Uiso 1 1 calc R . . H12C H 0.5421 0.5368 0.9197 0.132 Uiso 1 1 calc R . . C13 C 0.2911(5) 0.5285(4) 0.8155(4) 0.0907(19) Uani 1 1 d . . . H13A H 0.3181 0.5415 0.8588 0.136 Uiso 1 1 calc R . . H13B H 0.2343 0.5534 0.8125 0.136 Uiso 1 1 calc R . . H13C H 0.3267 0.5490 0.7796 0.136 Uiso 1 1 calc R . . C14 C 0.2381(5) 0.4140(6) 0.7252(4) 0.106(3) Uani 1 1 d . . . H14A H 0.2190 0.3586 0.7173 0.159 Uiso 1 1 calc R . . H14B H 0.2825 0.4279 0.6933 0.159 Uiso 1 1 calc R . . H14C H 0.1894 0.4506 0.7195 0.159 Uiso 1 1 calc R . . C15 C 0.4260(5) 0.1687(4) 0.8805(4) 0.097(2) Uani 1 1 d . . . H15A H 0.4715 0.1796 0.9138 0.145 Uiso 1 1 calc R . . H15B H 0.4516 0.1592 0.8369 0.145 Uiso 1 1 calc R . . H15C H 0.3938 0.1210 0.8938 0.145 Uiso 1 1 calc R . . C16 C 0.2631(5) 0.2066(5) 0.8333(4) 0.098(2) Uani 1 1 d . . . H16A H 0.2146 0.2440 0.8322 0.147 Uiso 1 1 calc R . . H16B H 0.2474 0.1579 0.8577 0.147 Uiso 1 1 calc R . . H16C H 0.2782 0.1924 0.7876 0.147 Uiso 1 1 calc R . . C17 C 0.4810(6) 0.5147(10) 0.6319(5) 0.173(6) Uani 1 1 d . . . H17A H 0.4329 0.4931 0.6053 0.260 Uiso 1 1 calc R . . H17B H 0.5275 0.5300 0.6024 0.260 Uiso 1 1 calc R . . H17C H 0.4619 0.5621 0.6566 0.260 Uiso 1 1 calc R . . C18 C 0.6207(4) 0.4853(6) 0.7107(4) 0.105(2) Uani 1 1 d . . . H18A H 0.6508 0.4517 0.7438 0.157 Uiso 1 1 calc R . . H18B H 0.6116 0.5390 0.7293 0.157 Uiso 1 1 calc R . . H18C H 0.6553 0.4896 0.6705 0.157 Uiso 1 1 calc R . . S20 S 0.0164(2) 0.22799(17) 0.73190(18) 0.1352(10) Uani 1 1 d . . . O21 O -0.0450(5) 0.1676(5) 0.7210(4) 0.146(2) Uani 1 1 d . . . O22 O 0.0237(7) 0.2797(7) 0.7840(5) 0.208(4) Uani 1 1 d . . . O23 O 0.1064(7) 0.1993(9) 0.7143(8) 0.286(7) Uani 1 1 d . . . C20 C 0.0157(8) 0.2907(7) 0.6598(7) 0.146(4) Uiso 1 1 d . . . F1 F 0.0161(7) 0.2511(6) 0.6062(5) 0.239(4) Uani 1 1 d . . . F2 F -0.0596(6) 0.3281(7) 0.6522(7) 0.245(4) Uani 1 1 d . . . F3 F 0.0679(5) 0.3494(5) 0.6544(5) 0.213(4) Uani 1 1 d . . . S30 S 0.26778(19) 0.49677(15) 0.50132(15) 0.1166(7) Uani 1 1 d . . . O31 O 0.2834(9) 0.4387(7) 0.5552(6) 0.247(5) Uani 1 1 d . . . O32 O 0.3176(10) 0.4859(10) 0.4495(7) 0.304(7) Uani 1 1 d . . . O33 O 0.2668(8) 0.5751(6) 0.5309(6) 0.226(5) Uani 1 1 d . . . C30 C 0.1600(10) 0.4675(9) 0.4838(8) 0.171(5) Uiso 1 1 d . . . F4 F 0.1476(7) 0.4043(6) 0.4512(6) 0.249(5) Uani 1 1 d . . . F5 F 0.1195(11) 0.4515(9) 0.5363(7) 0.319(7) Uani 1 1 d . . . F6 F 0.1134(11) 0.5228(9) 0.4579(9) 0.352(8) Uani 1 1 d . . . N50 N 0.8005(9) 0.3253(9) 0.0324(7) 0.185(5) Uiso 1 1 d . . . O50 O 0.8601(9) 0.3303(9) -0.0027(7) 0.229(5) Uiso 1 1 d . . . O51 O 0.7451(10) 0.3737(11) 0.0360(8) 0.261(7) Uiso 1 1 d . . . C50 C 0.7718(9) 0.2481(9) 0.0621(7) 0.167(5) Uiso 1 1 d . . . H50A H 0.7472 0.2584 0.1058 0.251 Uiso 1 1 calc R . . H50B H 0.8210 0.2118 0.0673 0.251 Uiso 1 1 calc R . . H50C H 0.7285 0.2233 0.0326 0.251 Uiso 1 1 calc R . . N40 N 0.7639(11) 0.3024(11) 0.8435(9) 0.205(6) Uiso 1 1 d . . . O40 O 0.7587(9) 0.3409(9) 0.7966(8) 0.235(6) Uiso 1 1 d . . . O41 O 0.7167(13) 0.3245(13) 0.8825(11) 0.315(9) Uiso 1 1 d . . . C40 C 0.7894(8) 0.2201(7) 0.8386(6) 0.141(4) Uiso 1 1 d . . . H40A H 0.7692 0.1904 0.8775 0.212 Uiso 1 1 calc R . . H40B H 0.8520 0.2169 0.8372 0.212 Uiso 1 1 calc R . . H40C H 0.7644 0.1966 0.7978 0.212 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 Ru1 0.0503(2) 0.0558(2) 0.0463(2) -0.00803(14) 0.00754(15) -0.00251(14) S1 0.0654(7) 0.0660(7) 0.0518(6) -0.0122(5) 0.0036(5) 0.0001(5) S2 0.0544(6) 0.0734(8) 0.0589(7) -0.0030(6) 0.0073(5) 0.0012(5) S3 0.0667(7) 0.0622(7) 0.0630(7) -0.0029(6) 0.0094(6) -0.0091(6) S4 0.0634(7) 0.0635(7) 0.0594(7) -0.0032(5) 0.0110(5) -0.0082(5) O4 0.091(3) 0.094(3) 0.087(3) 0.001(2) 0.040(2) -0.009(2) C1 0.093(4) 0.101(5) 0.067(3) -0.029(3) 0.008(3) 0.033(4) C2 0.081(4) 0.108(5) 0.081(4) -0.029(4) 0.007(3) 0.026(4) C3 0.055(3) 0.103(5) 0.099(5) 0.019(4) 0.005(3) -0.014(3) C4 0.065(3) 0.082(4) 0.119(5) 0.000(4) 0.016(3) -0.016(3) C5 0.113(5) 0.093(5) 0.067(4) 0.012(3) -0.002(3) -0.019(4) C6 0.102(4) 0.075(4) 0.062(3) -0.001(3) -0.009(3) 0.001(3) C7 0.106(5) 0.095(5) 0.085(5) 0.024(4) -0.007(4) -0.014(4) C8 0.110(5) 0.076(4) 0.090(5) -0.013(4) 0.005(4) -0.026(4) O1 0.0527(16) 0.068(2) 0.0521(17) -0.0116(15) 0.0012(13) 0.0052(14) O2 0.0569(17) 0.069(2) 0.0485(17) -0.0128(15) 0.0022(13) 0.0017(15) C9 0.056(2) 0.064(3) 0.045(2) -0.006(2) 0.0041(18) -0.011(2) C10 0.048(2) 0.061(3) 0.047(2) -0.0071(19) 0.0023(17) -0.0074(18) O8 0.0509(16) 0.070(2) 0.0509(17) -0.0164(15) 0.0022(13) 0.0015(14) O9 0.0558(17) 0.078(2) 0.0480(17) -0.0169(16) 0.0015(13) 0.0001(16) Ru2 0.0498(2) 0.0647(3) 0.0450(2) -0.01333(15) 0.00559(15) -0.00182(15) S5 0.0582(6) 0.0768(8) 0.0500(6) -0.0202(6) 0.0028(5) -0.0015(5) O5 0.072(2) 0.104(3) 0.060(2) -0.034(2) 0.0065(17) 0.007(2) S6 0.0556(6) 0.0805(9) 0.0601(7) -0.0151(6) 0.0040(5) 0.0064(6) O6 0.058(2) 0.125(4) 0.093(3) -0.008(3) 0.021(2) 0.009(2) S7 0.0693(7) 0.0738(8) 0.0568(7) -0.0104(6) 0.0162(6) -0.0076(6) O7 0.081(3) 0.100(3) 0.063(2) -0.010(2) 0.0236(19) -0.013(2) S8 0.0903(10) 0.0846(10) 0.0642(8) -0.0103(7) 0.0208(7) -0.0161(8) O3 0.073(2) 0.070(2) 0.060(2) -0.0074(17) 0.0114(16) -0.0061(17) C11 0.078(4) 0.112(5) 0.063(3) -0.019(3) -0.017(3) 0.017(3) C12 0.084(4) 0.112(5) 0.069(4) -0.028(4) 0.004(3) -0.034(4) C13 0.082(4) 0.081(4) 0.109(5) -0.013(4) 0.001(4) 0.011(3) C14 0.086(4) 0.155(7) 0.075(4) -0.033(5) -0.025(3) 0.038(5) C15 0.119(6) 0.081(4) 0.090(5) 0.013(4) 0.031(4) 0.013(4) C16 0.097(5) 0.103(5) 0.094(5) -0.027(4) 0.020(4) -0.035(4) C17 0.102(6) 0.325(19) 0.092(6) 0.086(9) 0.000(5) -0.010(8) C18 0.076(4) 0.127(6) 0.112(6) -0.017(5) 0.025(4) -0.022(4) S20 0.141(2) 0.1008(16) 0.162(3) -0.0371(16) -0.0442(18) -0.0038(14) O21 0.168(6) 0.129(5) 0.138(5) -0.004(4) -0.015(4) -0.027(4) O22 0.243(8) 0.206(8) 0.174(7) -0.063(7) -0.006(6) -0.009(7) O23 0.231(9) 0.293(10) 0.333(11) -0.027(9) -0.009(8) 0.037(8) F1 0.272(8) 0.259(8) 0.188(7) -0.025(6) 0.057(6) -0.065(7) F2 0.195(7) 0.237(8) 0.302(9) 0.025(7) -0.048(7) -0.016(6) F3 0.182(6) 0.213(7) 0.243(7) 0.022(6) -0.007(5) -0.107(5) S30 0.1453(19) 0.0879(14) 0.1175(17) 0.0045(12) 0.0212(15) -0.0127(13) O31 0.263(9) 0.216(9) 0.258(9) 0.041(8) -0.045(8) -0.043(7) O32 0.269(10) 0.372(12) 0.273(11) -0.026(9) 0.073(8) -0.023(9) O33 0.220(8) 0.194(8) 0.264(9) -0.036(7) -0.026(7) -0.048(7) F4 0.237(7) 0.209(7) 0.300(9) -0.092(7) -0.066(7) -0.022(6) F5 0.285(9) 0.355(11) 0.319(10) 0.032(9) 0.052(8) -0.052(8) F6 0.330(11) 0.343(12) 0.382(12) 0.015(9) -0.037(9) 0.028(9) _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 O1 2.131(3) . ? Ru1 O2 2.135(3) . ? Ru1 S2 2.2789(13) . ? Ru1 S1 2.2826(13) . ? Ru1 S4 2.3069(14) . ? Ru1 S3 2.3268(14) . ? S1 C1 1.822(6) . ? S1 C6 1.825(7) . ? S2 C2 1.825(7) . ? S2 C3 1.828(6) . ? S3 C4 1.809(7) . ? S3 C5 1.841(7) . ? S4 O4 1.477(4) . ? S4 C8 1.767(7) . ? S4 C7 1.769(7) . ? C1 C2 1.458(10) . ? C3 C4 1.488(10) . ? C5 C6 1.479(9) . ? O1 C9 1.262(6) . ? O2 C10 1.247(5) . ? C9 O9 1.248(6) . ? C9 C10 1.553(7) . ? C10 O8 1.257(5) . ? O8 Ru2 2.138(3) . ? O9 Ru2 2.117(3) . ? Ru2 O3 2.140(4) . ? Ru2 S7 2.2457(15) . ? Ru2 S5 2.2477(13) . ? Ru2 S6 2.2599(14) . ? S5 O5 1.476(4) . ? S5 C12 1.774(6) . ? S5 C11 1.793(7) . ? S6 O6 1.488(4) . ? S6 C14 1.738(7) . ? S6 C13 1.742(7) . ? S7 O7 1.478(4) . ? S7 C15 1.773(7) . ? S7 C16 1.778(7) . ? S8 O3 1.533(4) . ? S8 C17 1.742(11) . ? S8 C18 1.769(7) . ? S20 O22 1.328(8) . ? S20 O21 1.374(7) . ? S20 O23 1.499(10) . ? S20 C20 1.747(14) . ? C20 F1 1.234(11) . ? C20 F3 1.252(11) . ? C20 F2 1.307(11) . ? S30 O32 1.295(10) . ? S30 O33 1.403(10) . ? S30 O31 1.436(10) . ? S30 C30 1.743(16) . ? C30 F4 1.226(12) . ? C30 F5 1.240(12) . ? C30 F6 1.250(13) . ? N50 O50 1.156(12) . ? N50 O51 1.160(13) . ? N50 C50 1.457(18) . ? N40 O40 1.116(14) . ? N40 O41 1.122(14) . ? N40 C40 1.401(17) . ? 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 O1 Ru1 O2 79.17(12) . . ? O1 Ru1 S2 95.89(9) . . ? O2 Ru1 S2 173.99(10) . . ? O1 Ru1 S1 174.78(10) . . ? O2 Ru1 S1 96.53(9) . . ? S2 Ru1 S1 88.22(5) . . ? O1 Ru1 S4 84.92(10) . . ? O2 Ru1 S4 87.02(10) . . ? S2 Ru1 S4 96.01(5) . . ? S1 Ru1 S4 97.88(5) . . ? O1 Ru1 S3 88.52(10) . . ? O2 Ru1 S3 87.68(11) . . ? S2 Ru1 S3 88.78(5) . . ? S1 Ru1 S3 88.35(5) . . ? S4 Ru1 S3 172.24(5) . . ? C1 S1 C6 101.3(3) . . ? C1 S1 Ru1 106.4(2) . . ? C6 S1 Ru1 103.6(2) . . ? C2 S2 C3 98.7(4) . . ? C2 S2 Ru1 104.8(2) . . ? C3 S2 Ru1 106.6(2) . . ? C4 S3 C5 100.7(4) . . ? C4 S3 Ru1 102.5(2) . . ? C5 S3 Ru1 105.8(2) . . ? O4 S4 C8 107.6(3) . . ? O4 S4 C7 106.7(4) . . ? C8 S4 C7 100.8(4) . . ? O4 S4 Ru1 113.5(2) . . ? C8 S4 Ru1 115.5(3) . . ? C7 S4 Ru1 111.7(2) . . ? C2 C1 S1 115.2(4) . . ? C1 C2 S2 115.0(5) . . ? C4 C3 S2 113.4(4) . . ? C3 C4 S3 116.7(4) . . ? C6 C5 S3 112.7(5) . . ? C5 C6 S1 116.1(5) . . ? C9 O1 Ru1 112.6(3) . . ? C10 O2 Ru1 112.8(3) . . ? O9 C9 O1 125.0(4) . . ? O9 C9 C10 117.5(4) . . ? O1 C9 C10 117.4(4) . . ? O2 C10 O8 125.3(4) . . ? O2 C10 C9 117.9(4) . . ? O8 C10 C9 116.9(4) . . ? C10 O8 Ru2 112.7(3) . . ? C9 O9 Ru2 113.6(3) . . ? O9 Ru2 O8 78.83(12) . . ? O9 Ru2 O3 88.72(15) . . ? O8 Ru2 O3 86.89(14) . . ? O9 Ru2 S7 92.30(11) . . ? O8 Ru2 S7 91.57(10) . . ? O3 Ru2 S7 177.95(11) . . ? O9 Ru2 S5 92.45(9) . . ? O8 Ru2 S5 170.82(9) . . ? O3 Ru2 S5 90.06(11) . . ? S7 Ru2 S5 91.67(5) . . ? O9 Ru2 S6 172.79(10) . . ? O8 Ru2 S6 95.22(9) . . ? O3 Ru2 S6 86.87(11) . . ? S7 Ru2 S6 91.94(6) . . ? S5 Ru2 S6 93.26(5) . . ? O5 S5 C12 108.5(3) . . ? O5 S5 C11 106.6(3) . . ? C12 S5 C11 98.9(4) . . ? O5 S5 Ru2 121.42(17) . . ? C12 S5 Ru2 108.9(2) . . ? C11 S5 Ru2 110.0(2) . . ? O6 S6 C14 106.5(4) . . ? O6 S6 C13 107.6(3) . . ? C14 S6 C13 101.1(4) . . ? O6 S6 Ru2 118.7(2) . . ? C14 S6 Ru2 108.3(2) . . ? C13 S6 Ru2 113.0(2) . . ? O7 S7 C15 105.0(3) . . ? O7 S7 C16 108.2(3) . . ? C15 S7 C16 99.5(4) . . ? O7 S7 Ru2 118.1(2) . . ? C15 S7 Ru2 112.0(2) . . ? C16 S7 Ru2 112.2(3) . . ? O3 S8 C17 103.2(4) . . ? O3 S8 C18 106.2(3) . . ? C17 S8 C18 98.1(5) . . ? S8 O3 Ru2 124.6(2) . . ? O22 S20 O21 128.4(6) . . ? O22 S20 O23 108.2(7) . . ? O21 S20 O23 111.6(6) . . ? O22 S20 C20 104.6(7) . . ? O21 S20 C20 107.5(5) . . ? O23 S20 C20 89.2(8) . . ? F1 C20 F3 108.3(11) . . ? F1 C20 F2 99.7(11) . . ? F3 C20 F2 101.3(10) . . ? F1 C20 S20 112.6(10) . . ? F3 C20 S20 121.5(10) . . ? F2 C20 S20 110.8(10) . . ? O32 S30 O33 117.4(8) . . ? O32 S30 O31 113.4(9) . . ? O33 S30 O31 107.4(7) . . ? O32 S30 C30 112.2(9) . . ? O33 S30 C30 108.2(7) . . ? O31 S30 C30 96.1(7) . . ? F4 C30 F5 100.5(13) . . ? F4 C30 F6 108.3(14) . . ? F5 C30 F6 101.6(13) . . ? F4 C30 S30 117.9(12) . . ? F5 C30 S30 112.3(13) . . ? F6 C30 S30 114.2(13) . . ? O50 N50 O51 124.9(19) . . ? O50 N50 C50 123.1(16) . . ? O51 N50 C50 109.7(16) . . ? O40 N40 O41 110(2) . . ? O40 N40 C40 119.9(19) . . ? O41 N40 C40 123(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ru1 S1 C1 142.0(11) . . . . ? O2 Ru1 S1 C1 176.3(3) . . . . ? S2 Ru1 S1 C1 0.0(3) . . . . ? S4 Ru1 S1 C1 -95.8(3) . . . . ? S3 Ru1 S1 C1 88.8(3) . . . . ? O1 Ru1 S1 C6 35.7(11) . . . . ? O2 Ru1 S1 C6 70.0(3) . . . . ? S2 Ru1 S1 C6 -106.3(2) . . . . ? S4 Ru1 S1 C6 157.8(2) . . . . ? S3 Ru1 S1 C6 -17.5(2) . . . . ? O1 Ru1 S2 C2 167.9(3) . . . . ? O2 Ru1 S2 C2 -157.7(10) . . . . ? S1 Ru1 S2 C2 -15.4(3) . . . . ? S4 Ru1 S2 C2 82.4(3) . . . . ? S3 Ru1 S2 C2 -103.8(3) . . . . ? O1 Ru1 S2 C3 -88.1(3) . . . . ? O2 Ru1 S2 C3 -53.6(10) . . . . ? S1 Ru1 S2 C3 88.7(3) . . . . ? S4 Ru1 S2 C3 -173.6(3) . . . . ? S3 Ru1 S2 C3 0.3(3) . . . . ? O1 Ru1 S3 C4 79.4(3) . . . . ? O2 Ru1 S3 C4 158.6(3) . . . . ? S2 Ru1 S3 C4 -16.6(3) . . . . ? S1 Ru1 S3 C4 -104.8(3) . . . . ? S4 Ru1 S3 C4 111.7(5) . . . . ? O1 Ru1 S3 C5 -175.5(3) . . . . ? O2 Ru1 S3 C5 -96.3(3) . . . . ? S2 Ru1 S3 C5 88.5(3) . . . . ? S1 Ru1 S3 C5 0.3(3) . . . . ? S4 Ru1 S3 C5 -143.2(5) . . . . ? O1 Ru1 S4 O4 59.1(3) . . . . ? O2 Ru1 S4 O4 -20.3(3) . . . . ? S2 Ru1 S4 O4 154.5(2) . . . . ? S1 Ru1 S4 O4 -116.5(2) . . . . ? S3 Ru1 S4 O4 26.7(5) . . . . ? O1 Ru1 S4 C8 -175.9(3) . . . . ? O2 Ru1 S4 C8 104.7(3) . . . . ? S2 Ru1 S4 C8 -80.5(3) . . . . ? S1 Ru1 S4 C8 8.5(3) . . . . ? S3 Ru1 S4 C8 151.6(5) . . . . ? O1 Ru1 S4 C7 -61.6(3) . . . . ? O2 Ru1 S4 C7 -141.0(3) . . . . ? S2 Ru1 S4 C7 33.8(3) . . . . ? S1 Ru1 S4 C7 122.9(3) . . . . ? S3 Ru1 S4 C7 -94.0(5) . . . . ? C6 S1 C1 C2 128.7(6) . . . . ? Ru1 S1 C1 C2 20.7(7) . . . . ? S1 C1 C2 S2 -36.3(8) . . . . ? C3 S2 C2 C1 -76.6(6) . . . . ? Ru1 S2 C2 C1 33.3(6) . . . . ? C2 S2 C3 C4 129.4(6) . . . . ? Ru1 S2 C3 C4 21.1(6) . . . . ? S2 C3 C4 S3 -39.0(8) . . . . ? C5 S3 C4 C3 -73.1(7) . . . . ? Ru1 S3 C4 C3 35.9(6) . . . . ? C4 S3 C5 C6 128.8(6) . . . . ? Ru1 S3 C5 C6 22.4(6) . . . . ? S3 C5 C6 S1 -41.1(8) . . . . ? C1 S1 C6 C5 -71.6(6) . . . . ? Ru1 S1 C6 C5 38.5(6) . . . . ? O2 Ru1 O1 C9 -1.0(3) . . . . ? S2 Ru1 O1 C9 175.5(3) . . . . ? S1 Ru1 O1 C9 33.7(12) . . . . ? S4 Ru1 O1 C9 -88.9(3) . . . . ? S3 Ru1 O1 C9 86.9(3) . . . . ? O1 Ru1 O2 C10 -1.2(3) . . . . ? S2 Ru1 O2 C10 -36.2(12) . . . . ? S1 Ru1 O2 C10 -178.2(3) . . . . ? S4 Ru1 O2 C10 84.2(3) . . . . ? S3 Ru1 O2 C10 -90.1(3) . . . . ? Ru1 O1 C9 O9 -175.4(4) . . . . ? Ru1 O1 C9 C10 2.7(5) . . . . ? Ru1 O2 C10 O8 -176.1(4) . . . . ? Ru1 O2 C10 C9 2.8(5) . . . . ? O9 C9 C10 O2 174.3(4) . . . . ? O1 C9 C10 O2 -3.9(7) . . . . ? O9 C9 C10 O8 -6.7(7) . . . . ? O1 C9 C10 O8 175.1(4) . . . . ? O2 C10 O8 Ru2 -173.0(4) . . . . ? C9 C10 O8 Ru2 8.1(5) . . . . ? O1 C9 O9 Ru2 179.4(4) . . . . ? C10 C9 O9 Ru2 1.3(6) . . . . ? C9 O9 Ru2 O8 2.1(3) . . . . ? C9 O9 Ru2 O3 -85.0(4) . . . . ? C9 O9 Ru2 S7 93.3(3) . . . . ? C9 O9 Ru2 S5 -175.0(3) . . . . ? C9 O9 Ru2 S6 -32.7(11) . . . . ? C10 O8 Ru2 O9 -5.8(3) . . . . ? C10 O8 Ru2 O3 83.5(3) . . . . ? C10 O8 Ru2 S7 -97.8(3) . . . . ? C10 O8 Ru2 S5 12.8(9) . . . . ? C10 O8 Ru2 S6 170.1(3) . . . . ? O9 Ru2 S5 O5 -164.2(3) . . . . ? O8 Ru2 S5 O5 177.6(7) . . . . ? O3 Ru2 S5 O5 107.1(3) . . . . ? S7 Ru2 S5 O5 -71.8(2) . . . . ? S6 Ru2 S5 O5 20.2(2) . . . . ? O9 Ru2 S5 C12 68.7(3) . . . . ? O8 Ru2 S5 C12 50.5(7) . . . . ? O3 Ru2 S5 C12 -20.0(3) . . . . ? S7 Ru2 S5 C12 161.1(3) . . . . ? S6 Ru2 S5 C12 -106.9(3) . . . . ? O9 Ru2 S5 C11 -38.8(3) . . . . ? O8 Ru2 S5 C11 -57.0(7) . . . . ? O3 Ru2 S5 C11 -127.5(3) . . . . ? S7 Ru2 S5 C11 53.6(3) . . . . ? S6 Ru2 S5 C11 145.7(3) . . . . ? O9 Ru2 S6 O6 139.2(9) . . . . ? O8 Ru2 S6 O6 105.0(3) . . . . ? O3 Ru2 S6 O6 -168.5(3) . . . . ? S7 Ru2 S6 O6 13.2(2) . . . . ? S5 Ru2 S6 O6 -78.6(2) . . . . ? O9 Ru2 S6 C14 17.8(9) . . . . ? O8 Ru2 S6 C14 -16.4(4) . . . . ? O3 Ru2 S6 C14 70.2(4) . . . . ? S7 Ru2 S6 C14 -108.2(4) . . . . ? S5 Ru2 S6 C14 160.0(4) . . . . ? O9 Ru2 S6 C13 -93.4(9) . . . . ? O8 Ru2 S6 C13 -127.6(3) . . . . ? O3 Ru2 S6 C13 -41.0(3) . . . . ? S7 Ru2 S6 C13 140.6(3) . . . . ? S5 Ru2 S6 C13 48.8(3) . . . . ? O9 Ru2 S7 O7 115.7(2) . . . . ? O8 Ru2 S7 O7 -165.4(2) . . . . ? O3 Ru2 S7 O7 -124(3) . . . . ? S5 Ru2 S7 O7 23.2(2) . . . . ? S6 Ru2 S7 O7 -70.1(2) . . . . ? O9 Ru2 S7 C15 -6.4(3) . . . . ? O8 Ru2 S7 C15 72.5(3) . . . . ? O3 Ru2 S7 C15 114(3) . . . . ? S5 Ru2 S7 C15 -98.9(3) . . . . ? S6 Ru2 S7 C15 167.8(3) . . . . ? O9 Ru2 S7 C16 -117.2(3) . . . . ? O8 Ru2 S7 C16 -38.4(3) . . . . ? O3 Ru2 S7 C16 3(3) . . . . ? S5 Ru2 S7 C16 150.2(3) . . . . ? S6 Ru2 S7 C16 56.9(3) . . . . ? C17 S8 O3 Ru2 142.3(5) . . . . ? C18 S8 O3 Ru2 -115.0(4) . . . . ? O9 Ru2 O3 S8 39.0(3) . . . . ? O8 Ru2 O3 S8 -39.9(3) . . . . ? S7 Ru2 O3 S8 -81(3) . . . . ? S5 Ru2 O3 S8 131.4(3) . . . . ? S6 Ru2 O3 S8 -135.3(3) . . . . ? O22 S20 C20 F1 174.7(10) . . . . ? O21 S20 C20 F1 -46.4(11) . . . . ? O23 S20 C20 F1 66.0(11) . . . . ? O22 S20 C20 F3 43.9(12) . . . . ? O21 S20 C20 F3 -177.2(10) . . . . ? O23 S20 C20 F3 -64.8(11) . . . . ? O22 S20 C20 F2 -74.7(10) . . . . ? O21 S20 C20 F2 64.3(10) . . . . ? O23 S20 C20 F2 176.7(10) . . . . ? O32 S30 C30 F4 41.3(15) . . . . ? O33 S30 C30 F4 172.4(12) . . . . ? O31 S30 C30 F4 -77.0(13) . . . . ? O32 S30 C30 F5 157.5(13) . . . . ? O33 S30 C30 F5 -71.4(13) . . . . ? O31 S30 C30 F5 39.2(13) . . . . ? O32 S30 C30 F6 -87.5(15) . . . . ? O33 S30 C30 F6 43.6(15) . . . . ? O31 S30 C30 F6 154.2(14) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.313 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.169 #===END