# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Ioannis Bratsos' _publ_contact_author_email 'jbratsos@units.it, bratsos@chem.demokritos.gr' loop_ _publ_author_name 'Ana Rilak' 'Ioannis Bratsos' 'Ennio Zangrando' 'Jakob Kljun' 'Iztok Turel' 'Zivadin Bugarcic' 'Enzo Alessio' data_2 _database_code_depnum_ccdc_archive 'CCDC 886390' #TrackingRef '- data2-4-10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H20 Cl N2 Ru S3 1+, P F6 1-' _chemical_formula_sum 'C16 H20 Cl F6 N2 P Ru S3' _chemical_formula_weight 618.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 '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' _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 16.6200(14) _cell_length_b 9.6130(9) _cell_length_c 14.6900(11) _cell_angle_alpha 90.00 _cell_angle_beta 111.888(9) _cell_angle_gamma 90.00 _cell_volume 2177.8(3) _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 block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 1.262 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6210 _exptl_absorpt_correction_T_max 0.7140 _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 'Enraf-Nonius dip1030 image plate diffractometer' _diffrn_measurement_method '\f-scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33504 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 26.42 _reflns_number_total 4301 _reflns_number_gt 3347 _reflns_threshold_expression >2\s(I) _computing_data_collection 'XPRESS (MacScience, 2002)' _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Scala (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.80.05 (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^ > 2\s(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^)+(0.0640P)^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 SHELXL _refine_ls_extinction_coef 0.0043(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4301 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 0.793609(16) 0.22442(3) 0.855496(18) 0.04185(12) Uani 1 1 d . . . Cl Cl 0.83510(6) 0.38597(11) 0.75309(6) 0.0573(2) Uani 1 1 d . . . S3 S 0.74455(6) 0.07151(10) 0.94199(6) 0.0514(2) Uani 1 1 d . . . S1 S 0.66004(5) 0.21012(10) 0.73069(6) 0.0476(2) Uani 1 1 d . . . S2 S 0.73796(6) 0.40282(10) 0.91880(7) 0.0521(2) Uani 1 1 d . . . N1 N 0.92247(19) 0.2395(3) 0.9556(2) 0.0476(7) Uani 1 1 d . . . N2 N 0.85570(17) 0.0691(3) 0.80605(19) 0.0461(6) Uani 1 1 d . . . C1 C 0.9531(3) 0.3302(5) 1.0307(3) 0.0613(10) Uani 1 1 d . . . H1 H 0.9136 0.3821 1.0477 0.074 Uiso 1 1 calc R . . C2 C 1.0396(3) 0.3491(5) 1.0828(3) 0.0694(11) Uani 1 1 d . . . H2 H 1.0581 0.4131 1.1340 0.083 Uiso 1 1 calc R . . C3 C 1.0989(3) 0.2738(5) 1.0596(3) 0.0696(12) Uani 1 1 d . . . H3 H 1.1580 0.2856 1.0945 0.084 Uiso 1 1 calc R . . C4 C 1.0693(2) 0.1800(5) 0.9835(3) 0.0607(10) Uani 1 1 d . . . H4 H 1.1086 0.1272 0.9666 0.073 Uiso 1 1 calc R . . C5 C 0.9809(2) 0.1645(4) 0.9319(2) 0.0503(8) Uani 1 1 d . . . C6 C 0.9433(2) 0.0679(4) 0.8489(2) 0.0487(8) Uani 1 1 d . . . C7 C 0.9926(2) -0.0190(5) 0.8152(3) 0.0626(10) Uani 1 1 d . . . H7 H 1.0528 -0.0173 0.8447 0.075 Uiso 1 1 calc R . . C8 C 0.9526(3) -0.1077(5) 0.7383(3) 0.0715(12) Uani 1 1 d . . . H8 H 0.9853 -0.1655 0.7148 0.086 Uiso 1 1 calc R . . C9 C 0.8638(3) -0.1101(5) 0.6966(3) 0.0688(11) Uani 1 1 d . . . H09 H 0.8352 -0.1713 0.6458 0.083 Uiso 1 1 calc R . . C10 C 0.8179(2) -0.0198(4) 0.7318(2) 0.0547(9) Uani 1 1 d . . . H10 H 0.7577 -0.0204 0.7027 0.066 Uiso 1 1 calc R . . C11 C 0.6513(2) -0.0113(4) 0.8470(3) 0.0625(10) Uani 1 1 d . . . H11A H 0.6722 -0.0813 0.8137 0.075 Uiso 1 1 calc R . . H11B H 0.6165 -0.0580 0.8781 0.075 Uiso 1 1 calc R . . C12 C 0.5946(2) 0.0909(4) 0.7720(3) 0.0588(10) Uani 1 1 d . . . H12A H 0.5603 0.1440 0.8006 0.071 Uiso 1 1 calc R . . H12B H 0.5551 0.0403 0.7161 0.071 Uiso 1 1 calc R . . C13 C 0.6098(3) 0.3774(4) 0.7328(3) 0.0620(10) Uani 1 1 d . . . H13A H 0.6315 0.4450 0.6985 0.074 Uiso 1 1 calc R . . H13B H 0.5478 0.3692 0.6974 0.074 Uiso 1 1 calc R . . C14 C 0.6260(3) 0.4305(5) 0.8334(3) 0.0741(12) Uani 1 1 d . . . H14A H 0.5868 0.3841 0.8588 0.089 Uiso 1 1 calc R . . H14B H 0.6131 0.5292 0.8298 0.089 Uiso 1 1 calc R . . C15 C 0.7198(3) 0.3199(5) 1.0215(3) 0.0741(12) Uani 1 1 d . . . H15A H 0.7739 0.3212 1.0781 0.089 Uiso 1 1 calc R . . H15B H 0.6782 0.3752 1.0377 0.089 Uiso 1 1 calc R . . C16 C 0.6882(3) 0.1756(5) 1.0046(3) 0.0614(10) Uani 1 1 d . . . H16A H 0.6266 0.1761 0.9653 0.074 Uiso 1 1 calc R . . H16B H 0.6961 0.1326 1.0671 0.074 Uiso 1 1 calc R . . P P 0.59674(8) 0.75723(12) 0.56303(10) 0.0673(3) Uani 1 1 d . . . F1 F 0.6715(4) 0.7337(6) 0.6691(4) 0.151(3) Uani 0.804(7) 1 d P A . F2 F 0.6129(4) 0.9153(4) 0.5906(4) 0.1258(19) Uani 0.804(7) 1 d P A . F3 F 0.6698(6) 0.7727(9) 0.5181(7) 0.205(4) Uani 0.804(7) 1 d P A . F4 F 0.5910(5) 0.6015(4) 0.5359(4) 0.158(3) Uani 0.804(7) 1 d P A . F5 F 0.5290(6) 0.7772(8) 0.4625(6) 0.206(5) Uani 0.804(7) 1 d P A . F6 F 0.5341(5) 0.7444(11) 0.6152(9) 0.218(5) Uani 0.804(7) 1 d P A . F2A F 0.5021(11) 0.8319(19) 0.5337(16) 0.094(5) Uiso 0.196(7) 1 d P A 2 F3A F 0.5758(15) 0.791(2) 0.4499(16) 0.088(6) Uiso 0.196(7) 1 d P A 2 F1A F 0.6682(11) 0.667(2) 0.5746(12) 0.088(5) Uiso 0.196(7) 1 d P A 2 F4A F 0.5948(18) 0.735(2) 0.6661(15) 0.103(6) Uiso 0.196(7) 1 d P A 2 F5A F 0.5475(19) 0.625(3) 0.584(2) 0.163(11) Uiso 0.196(7) 1 d P A 2 F6A F 0.6452(13) 0.875(3) 0.5514(17) 0.112(7) Uiso 0.196(7) 1 d P A 2 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 0.03608(17) 0.0491(2) 0.04023(17) -0.00165(10) 0.01409(12) -0.00024(11) Cl 0.0502(5) 0.0675(6) 0.0545(5) 0.0046(4) 0.0198(4) -0.0110(4) S3 0.0508(5) 0.0566(6) 0.0489(5) 0.0058(4) 0.0212(4) 0.0022(4) S1 0.0385(4) 0.0609(6) 0.0421(4) -0.0017(3) 0.0136(3) -0.0011(4) S2 0.0512(5) 0.0538(6) 0.0523(5) -0.0059(4) 0.0205(4) 0.0025(4) N1 0.0429(16) 0.0496(18) 0.0470(16) -0.0015(12) 0.0131(13) -0.0037(12) N2 0.0381(14) 0.0504(18) 0.0491(15) 0.0004(12) 0.0156(12) 0.0006(12) C1 0.062(2) 0.061(3) 0.054(2) -0.0089(18) 0.0127(18) -0.003(2) C2 0.061(2) 0.065(3) 0.061(2) -0.0034(19) -0.0022(19) -0.012(2) C3 0.045(2) 0.071(3) 0.077(3) 0.013(2) 0.004(2) -0.009(2) C4 0.0390(19) 0.068(3) 0.066(2) 0.012(2) 0.0099(17) -0.0010(18) C5 0.0441(18) 0.055(2) 0.0526(19) 0.0083(16) 0.0188(15) -0.0014(16) C6 0.0431(18) 0.051(2) 0.0541(19) 0.0048(15) 0.0207(15) -0.0006(15) C7 0.048(2) 0.071(3) 0.075(2) 0.001(2) 0.0304(18) 0.0068(19) C8 0.067(3) 0.078(3) 0.081(3) -0.010(2) 0.040(2) 0.013(2) C9 0.070(3) 0.072(3) 0.070(2) -0.020(2) 0.033(2) 0.001(2) C10 0.0453(19) 0.066(3) 0.0522(18) -0.0023(17) 0.0170(15) 0.0023(17) C11 0.064(2) 0.061(3) 0.067(2) -0.0023(19) 0.0298(19) -0.014(2) C12 0.0404(19) 0.071(3) 0.065(2) -0.0054(18) 0.0198(17) -0.0125(18) C13 0.057(2) 0.069(3) 0.056(2) 0.0079(18) 0.0160(17) 0.014(2) C14 0.064(3) 0.077(3) 0.077(3) -0.002(2) 0.020(2) 0.022(2) C15 0.086(3) 0.090(3) 0.057(2) -0.013(2) 0.039(2) -0.001(3) C16 0.065(2) 0.080(3) 0.0475(19) -0.0013(18) 0.0311(18) 0.001(2) P 0.0724(8) 0.0574(7) 0.0734(7) -0.0104(5) 0.0286(6) -0.0061(5) F1 0.126(5) 0.149(5) 0.125(4) 0.041(3) -0.016(3) -0.024(3) F2 0.154(4) 0.064(3) 0.138(4) -0.037(2) 0.029(3) -0.013(3) F3 0.241(10) 0.224(8) 0.238(10) -0.066(6) 0.191(9) -0.071(6) F4 0.301(9) 0.058(3) 0.155(4) -0.027(3) 0.132(6) -0.016(4) F5 0.188(8) 0.180(7) 0.129(6) 0.028(5) -0.081(6) -0.051(6) F6 0.123(6) 0.336(13) 0.255(11) -0.093(9) 0.141(7) -0.060(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N2 2.093(3) . ? Ru N1 2.103(3) . ? Ru S3 2.2830(9) . ? Ru S1 2.2965(9) . ? Ru S2 2.3027(9) . ? Ru Cl 2.4338(9) . ? S3 C16 1.834(4) . ? S3 C11 1.835(4) . ? S1 C13 1.818(4) . ? S1 C12 1.831(4) . ? S2 C15 1.828(4) . ? S2 C14 1.835(4) . ? N1 C1 1.347(5) . ? N1 C5 1.356(4) . ? N2 C10 1.343(4) . ? N2 C6 1.353(4) . ? C1 C2 1.367(5) . ? C1 H1 0.9300 . ? C2 C3 1.365(6) . ? C2 H2 0.9300 . ? C3 C4 1.377(6) . ? C3 H3 0.9300 . ? C4 C5 1.388(5) . ? C4 H4 0.9300 . ? C5 C6 1.474(5) . ? C6 C7 1.384(5) . ? C7 C8 1.373(6) . ? C7 H7 0.9300 . ? C8 C9 1.371(6) . ? C8 H8 0.9300 . ? C9 C10 1.377(5) . ? C9 H09 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.514(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.490(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.471(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? P F5 1.499(6) . ? P F6 1.511(6) . ? P F4 1.543(4) . ? P F2 1.570(4) . ? P F3 1.590(6) . ? P F1 1.606(5) . ? P F1A 1.427(16) . ? P F6A 1.43(2) . ? P F4A 1.54(2) . ? P F3A 1.60(2) . ? P F5A 1.60(3) . ? P F2A 1.633(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 N2 Ru N1 77.68(11) . . ? N2 Ru S3 93.35(8) . . ? N1 Ru S3 97.87(8) . . ? N2 Ru S1 97.77(8) . . ? N1 Ru S1 172.67(8) . . ? S3 Ru S1 88.07(3) . . ? N2 Ru S2 174.65(8) . . ? N1 Ru S2 97.11(8) . . ? S3 Ru S2 88.52(4) . . ? S1 Ru S2 87.29(3) . . ? N2 Ru Cl 87.17(8) . . ? N1 Ru Cl 86.51(8) . . ? S3 Ru Cl 175.61(3) . . ? S1 Ru Cl 87.54(3) . . ? S2 Ru Cl 91.34(4) . . ? C16 S3 C11 99.97(18) . . ? C16 S3 Ru 106.41(14) . . ? C11 S3 Ru 103.40(13) . . ? C13 S1 C12 102.42(19) . . ? C13 S1 Ru 104.29(13) . . ? C12 S1 Ru 106.83(13) . . ? C15 S2 C14 100.9(2) . . ? C15 S2 Ru 102.90(16) . . ? C14 S2 Ru 106.83(14) . . ? C1 N1 C5 117.8(3) . . ? C1 N1 Ru 126.3(3) . . ? C5 N1 Ru 115.1(2) . . ? C10 N2 C6 117.9(3) . . ? C10 N2 Ru 126.5(2) . . ? C6 N2 Ru 115.4(2) . . ? N1 C1 C2 122.8(4) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.8(4) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 118.5(4) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C3 C4 C5 119.9(4) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? N1 C5 C4 121.1(4) . . ? N1 C5 C6 115.1(3) . . ? C4 C5 C6 123.8(3) . . ? N2 C6 C7 121.1(3) . . ? N2 C6 C5 115.5(3) . . ? C7 C6 C5 123.4(3) . . ? C8 C7 C6 119.9(4) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C9 C8 C7 119.3(4) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 118.4(4) . . ? C8 C9 H09 120.8 . . ? C10 C9 H09 120.8 . . ? N2 C10 C9 123.3(3) . . ? N2 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? C12 C11 S3 113.1(3) . . ? C12 C11 H11A 109.0 . . ? S3 C11 H11A 109.0 . . ? C12 C11 H11B 109.0 . . ? S3 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C12 S1 111.2(2) . . ? C11 C12 H12A 109.4 . . ? S1 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? S1 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C14 C13 S1 113.9(3) . . ? C14 C13 H13A 108.8 . . ? S1 C13 H13A 108.8 . . ? C14 C13 H13B 108.8 . . ? S1 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C13 C14 S2 113.0(3) . . ? C13 C14 H14A 109.0 . . ? S2 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? S2 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C16 C15 S2 115.4(3) . . ? C16 C15 H15A 108.4 . . ? S2 C15 H15A 108.4 . . ? C16 C15 H15B 108.4 . . ? S2 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? C15 C16 S3 112.5(3) . . ? C15 C16 H16A 109.1 . . ? S3 C16 H16A 109.1 . . ? C15 C16 H16B 109.1 . . ? S3 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? F5 P F6 95.9(6) . . ? F5 P F4 85.3(4) . . ? F6 P F4 93.7(4) . . ? F5 P F2 97.1(3) . . ? F6 P F2 91.8(5) . . ? F4 P F2 173.7(4) . . ? F5 P F3 89.3(5) . . ? F6 P F3 174.5(6) . . ? F4 P F3 88.1(4) . . ? F2 P F3 86.2(3) . . ? F5 P F1 178.1(6) . . ? F6 P F1 85.8(5) . . ? F4 P F1 93.7(3) . . ? F2 P F1 83.7(3) . . ? F3 P F1 88.9(5) . . ? F1A P F6A 90.7(13) . . ? F1A P F4A 96.8(11) . . ? F6A P F4A 116.4(13) . . ? F1A P F3A 95.6(10) . . ? F6A P F3A 68.2(12) . . ? F4A P F3A 166.6(12) . . ? F1A P F5A 87.6(13) . . ? F6A P F5A 175.9(13) . . ? F4A P F5A 60.2(14) . . ? F3A P F5A 115.6(14) . . ? F1A P F2A 167.0(11) . . ? F6A P F2A 98.7(11) . . ? F4A P F2A 87.1(11) . . ? F3A P F2A 79.6(10) . . ? F5A P F2A 83.6(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru S3 C16 177.11(15) . . . . ? N1 Ru S3 C16 99.09(16) . . . . ? S1 Ru S3 C16 -85.22(14) . . . . ? S2 Ru S3 C16 2.12(14) . . . . ? Cl Ru S3 C16 -86.2(5) . . . . ? N2 Ru S3 C11 -78.07(16) . . . . ? N1 Ru S3 C11 -156.09(16) . . . . ? S1 Ru S3 C11 19.60(14) . . . . ? S2 Ru S3 C11 106.94(14) . . . . ? Cl Ru S3 C11 18.7(5) . . . . ? N2 Ru S1 C13 -158.38(15) . . . . ? N1 Ru S1 C13 -107.2(7) . . . . ? S3 Ru S1 C13 108.49(14) . . . . ? S2 Ru S1 C13 19.88(14) . . . . ? Cl Ru S1 C13 -71.58(14) . . . . ? N2 Ru S1 C12 93.63(16) . . . . ? N1 Ru S1 C12 144.8(7) . . . . ? S3 Ru S1 C12 0.50(14) . . . . ? S2 Ru S1 C12 -88.11(14) . . . . ? Cl Ru S1 C12 -179.57(14) . . . . ? N2 Ru S2 C15 -94.8(8) . . . . ? N1 Ru S2 C15 -81.88(18) . . . . ? S3 Ru S2 C15 15.87(16) . . . . ? S1 Ru S2 C15 104.00(16) . . . . ? Cl Ru S2 C15 -168.53(16) . . . . ? N2 Ru S2 C14 159.4(8) . . . . ? N1 Ru S2 C14 172.29(18) . . . . ? S3 Ru S2 C14 -89.96(17) . . . . ? S1 Ru S2 C14 -1.83(17) . . . . ? Cl Ru S2 C14 85.64(17) . . . . ? N2 Ru N1 C1 179.4(3) . . . . ? S3 Ru N1 C1 -88.9(3) . . . . ? S1 Ru N1 C1 127.2(6) . . . . ? S2 Ru N1 C1 0.6(3) . . . . ? Cl Ru N1 C1 91.5(3) . . . . ? N2 Ru N1 C5 10.0(2) . . . . ? S3 Ru N1 C5 101.7(2) . . . . ? S1 Ru N1 C5 -42.2(8) . . . . ? S2 Ru N1 C5 -168.8(2) . . . . ? Cl Ru N1 C5 -77.9(2) . . . . ? N1 Ru N2 C10 176.7(3) . . . . ? S3 Ru N2 C10 79.3(3) . . . . ? S1 Ru N2 C10 -9.2(3) . . . . ? S2 Ru N2 C10 -170.2(7) . . . . ? Cl Ru N2 C10 -96.3(3) . . . . ? N1 Ru N2 C6 -9.2(2) . . . . ? S3 Ru N2 C6 -106.5(2) . . . . ? S1 Ru N2 C6 165.0(2) . . . . ? S2 Ru N2 C6 3.9(10) . . . . ? Cl Ru N2 C6 77.9(2) . . . . ? C5 N1 C1 C2 0.1(6) . . . . ? Ru N1 C1 C2 -169.1(3) . . . . ? N1 C1 C2 C3 -0.3(7) . . . . ? C1 C2 C3 C4 0.0(7) . . . . ? C2 C3 C4 C5 0.4(6) . . . . ? C1 N1 C5 C4 0.4(5) . . . . ? Ru N1 C5 C4 170.7(3) . . . . ? C1 N1 C5 C6 -179.7(3) . . . . ? Ru N1 C5 C6 -9.3(4) . . . . ? C3 C4 C5 N1 -0.6(6) . . . . ? C3 C4 C5 C6 179.4(4) . . . . ? C10 N2 C6 C7 2.1(5) . . . . ? Ru N2 C6 C7 -172.6(3) . . . . ? C10 N2 C6 C5 -178.1(3) . . . . ? Ru N2 C6 C5 7.2(4) . . . . ? N1 C5 C6 N2 1.5(5) . . . . ? C4 C5 C6 N2 -178.6(3) . . . . ? N1 C5 C6 C7 -178.8(3) . . . . ? C4 C5 C6 C7 1.2(6) . . . . ? N2 C6 C7 C8 -1.2(6) . . . . ? C5 C6 C7 C8 179.0(4) . . . . ? C6 C7 C8 C9 -0.9(7) . . . . ? C7 C8 C9 C10 2.0(7) . . . . ? C6 N2 C10 C9 -0.9(6) . . . . ? Ru N2 C10 C9 173.1(3) . . . . ? C8 C9 C10 N2 -1.1(7) . . . . ? C16 S3 C11 C12 67.1(3) . . . . ? Ru S3 C11 C12 -42.6(3) . . . . ? S3 C11 C12 S1 45.7(4) . . . . ? C13 S1 C12 C11 -135.5(3) . . . . ? Ru S1 C12 C11 -26.2(3) . . . . ? C12 S1 C13 C14 70.9(3) . . . . ? Ru S1 C13 C14 -40.3(3) . . . . ? S1 C13 C14 S2 41.6(4) . . . . ? C15 S2 C14 C13 -129.2(4) . . . . ? Ru S2 C14 C13 -22.0(4) . . . . ? C14 S2 C15 C16 72.4(4) . . . . ? Ru S2 C15 C16 -37.9(4) . . . . ? S2 C15 C16 S3 42.8(4) . . . . ? C11 S3 C16 C15 -132.8(3) . . . . ? Ru S3 C16 C15 -25.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.616 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.076 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 886391' #TrackingRef '- data2-4-10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H27 N7 O Ru S3 2+, 2(P F6 1-), (H2 O)' _chemical_formula_sum 'C14 H29 F12 N7 O2 P2 Ru S3' _chemical_formula_weight 814.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 8.5941(2) _cell_length_b 11.3013(2) _cell_length_c 14.8054(3) _cell_angle_alpha 99.2630(10) _cell_angle_beta 91.0800(10) _cell_angle_gamma 92.0160(10) _cell_volume 1417.90(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.995 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8651 _exptl_absorpt_correction_T_max 0.9070 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11707 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.45 _reflns_number_total 6449 _reflns_number_gt 5570 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.80.05 (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^ > 2\s(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^)+(0.0184P)^2^+0.7856P] 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 6449 _refine_ls_number_parameters 386 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0612 _refine_ls_wR_factor_gt 0.0585 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _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 0.365365(18) 0.348062(14) 0.244986(11) 0.01111(5) Uani 1 1 d . . . S1 S 0.11059(6) 0.38793(5) 0.27687(3) 0.01458(11) Uani 1 1 d . . . S2 S 0.41740(6) 0.37866(5) 0.40008(3) 0.01544(11) Uani 1 1 d . . . S3 S 0.30879(6) 0.15066(4) 0.25186(3) 0.01528(11) Uani 1 1 d . . . O1 O 0.74750(17) 0.51001(13) 0.32398(10) 0.0207(3) Uani 1 1 d . . . N1 N 0.7778(2) 0.70830(16) 0.31523(13) 0.0203(4) Uani 1 1 d D . . H1 H 0.865(2) 0.705(2) 0.3401(16) 0.024(7) Uiso 1 1 d D . . N2 N 0.8345(2) 0.90847(18) 0.31154(15) 0.0321(5) Uani 1 1 d . . . H2A H 0.8113 0.9783 0.2969 0.038 Uiso 1 1 calc R . . H2B H 0.9239 0.9004 0.3394 0.038 Uiso 1 1 calc R . . C2 C 0.7335(3) 0.81452(19) 0.29158(15) 0.0214(5) Uani 1 1 d . . . N3 N 0.5995(2) 0.82663(15) 0.24994(13) 0.0202(4) Uani 1 1 d . . . C4 C 0.5094(2) 0.72394(18) 0.23648(14) 0.0152(4) Uani 1 1 d . . . C5 C 0.5436(2) 0.61282(18) 0.25808(14) 0.0144(4) Uani 1 1 d . . . C6 C 0.6913(2) 0.59865(18) 0.29987(14) 0.0159(4) Uani 1 1 d . . . N7 N 0.41423(19) 0.53402(14) 0.23579(11) 0.0130(3) Uani 1 1 d . . . C8 C 0.3094(2) 0.59911(18) 0.20243(14) 0.0157(4) Uani 1 1 d . . . H8 H 0.2079 0.5691 0.1823 0.019 Uiso 1 1 calc R . . N9 N 0.3615(2) 0.71325(15) 0.19985(12) 0.0159(4) Uani 1 1 d . . . C9 C 0.2725(3) 0.80772(19) 0.16889(16) 0.0217(5) Uani 1 1 d . . . H9A H 0.2517 0.8694 0.2213 0.033 Uiso 1 1 calc R . . H9B H 0.1736 0.7732 0.1406 0.033 Uiso 1 1 calc R . . H9C H 0.3325 0.8439 0.1240 0.033 Uiso 1 1 calc R . . N4 N 0.5995(2) 0.31040(16) 0.20594(12) 0.0178(4) Uani 1 1 d . . . H4A H 0.6681 0.3626 0.2423 0.021 Uiso 1 1 calc R . . H4B H 0.6213 0.2335 0.2136 0.021 Uiso 1 1 calc R . . N5 N 0.3339(2) 0.31760(16) 0.09781(11) 0.0168(4) Uani 1 1 d . . . H5A H 0.2492 0.2662 0.0811 0.020 Uiso 1 1 calc R . . H5B H 0.3159 0.3890 0.0778 0.020 Uiso 1 1 calc R . . C10 C 0.4764(3) 0.2647(2) 0.05518(16) 0.0270(5) Uani 1 1 d . . . H10A H 0.4811 0.2779 -0.0092 0.032 Uiso 1 1 calc R . . H10B H 0.4741 0.1772 0.0559 0.032 Uiso 1 1 calc R . . C11 C 0.6171(3) 0.3239(2) 0.10864(16) 0.0260(5) Uani 1 1 d . . . H11B H 0.7129 0.2856 0.0845 0.031 Uiso 1 1 calc R . . H11A H 0.6252 0.4100 0.1030 0.031 Uiso 1 1 calc R . . C12 C 0.0988(2) 0.4168(2) 0.40199(14) 0.0186(4) Uani 1 1 d . . . H12A H 0.0177 0.4756 0.4200 0.022 Uiso 1 1 calc R . . H12B H 0.0685 0.3415 0.4242 0.022 Uiso 1 1 calc R . . C13 C 0.2535(3) 0.4653(2) 0.44587(14) 0.0196(5) Uani 1 1 d . . . H13A H 0.2497 0.4651 0.5126 0.024 Uiso 1 1 calc R . . H13B H 0.2703 0.5494 0.4363 0.024 Uiso 1 1 calc R . . C14 C 0.3710(3) 0.23386(19) 0.43721(15) 0.0201(5) Uani 1 1 d . . . H14A H 0.4367 0.2261 0.4914 0.024 Uiso 1 1 calc R . . H14B H 0.2606 0.2308 0.4550 0.024 Uiso 1 1 calc R . . C15 C 0.3991(3) 0.13068(19) 0.36084(15) 0.0197(5) Uani 1 1 d . . . H15A H 0.3570 0.0552 0.3784 0.024 Uiso 1 1 calc R . . H15B H 0.5126 0.1231 0.3531 0.024 Uiso 1 1 calc R . . C16 C 0.1010(2) 0.14050(19) 0.27933(15) 0.0199(5) Uani 1 1 d . . . H16A H 0.0551 0.0626 0.2483 0.024 Uiso 1 1 calc R . . H16B H 0.0914 0.1430 0.3461 0.024 Uiso 1 1 calc R . . C17 C 0.0100(2) 0.24134(19) 0.25012(15) 0.0194(5) Uani 1 1 d . . . H17A H -0.0915 0.2449 0.2808 0.023 Uiso 1 1 calc R . . H17B H -0.0113 0.2229 0.1833 0.023 Uiso 1 1 calc R . . P1 P 0.18777(7) 0.82225(5) 0.46601(4) 0.02043(13) Uani 1 1 d . . . P2 P 0.0000 0.5000 0.0000 0.02459(19) Uani 1 2 d S . . P3 P 0.0000 0.0000 0.0000 0.02081(17) Uani 1 2 d S . . F1 F 0.33323(16) 0.76387(14) 0.41420(10) 0.0365(4) Uani 1 1 d . . . F2 F 0.0379(2) 0.87848(15) 0.51559(12) 0.0499(5) Uani 1 1 d . . . F3 F 0.22155(18) 0.75177(13) 0.54876(10) 0.0360(4) Uani 1 1 d . . . F4 F 0.15123(17) 0.89216(14) 0.38200(10) 0.0352(3) Uani 1 1 d . . . F5 F 0.07816(18) 0.71060(13) 0.41675(12) 0.0435(4) Uani 1 1 d . . . F6 F 0.2952(2) 0.93241(13) 0.51328(11) 0.0430(4) Uani 1 1 d . . . F7 F 0.18631(16) 0.52116(14) 0.01021(10) 0.0337(3) Uani 1 1 d . . . F8 F -0.02093(19) 0.59288(16) 0.09123(11) 0.0505(4) Uani 1 1 d . . . F9 F 0.01051(18) 0.39443(15) 0.05900(12) 0.0470(4) Uani 1 1 d . . . F10 F 0.13046(19) 0.08968(15) 0.05372(11) 0.0469(4) Uani 1 1 d . . . F11 F -0.12866(19) 0.09583(14) 0.03001(11) 0.0446(4) Uani 1 1 d . . . F12 F -0.0302(2) -0.05557(14) 0.09080(10) 0.0419(4) Uani 1 1 d . . . O1w O 0.6647(2) 0.05151(16) 0.18431(15) 0.0346(5) Uani 1 1 d . . . H1B H 0.620(4) -0.013(3) 0.187(2) 0.055(10) Uiso 1 1 d . . . H1A H 0.721(4) 0.035(3) 0.145(2) 0.036(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.00977(9) 0.01096(8) 0.01304(8) 0.00334(6) 0.00023(6) 0.00012(6) S1 0.0109(2) 0.0183(2) 0.0146(2) 0.0029(2) 0.00009(19) 0.0012(2) S2 0.0134(2) 0.0172(2) 0.0157(2) 0.0030(2) -0.00264(19) -0.0001(2) S3 0.0153(3) 0.0127(2) 0.0181(3) 0.00366(19) 0.0005(2) -0.0015(2) O1 0.0165(8) 0.0210(8) 0.0267(8) 0.0103(7) -0.0046(6) 0.0009(6) N1 0.0150(9) 0.0197(9) 0.0273(10) 0.0087(8) -0.0065(8) -0.0035(8) N2 0.0242(11) 0.0216(10) 0.0513(14) 0.0122(10) -0.0113(10) -0.0092(9) C2 0.0202(11) 0.0192(11) 0.0252(12) 0.0057(9) -0.0005(9) -0.0047(9) N3 0.0200(10) 0.0138(9) 0.0274(10) 0.0067(8) -0.0022(8) -0.0037(7) C4 0.0155(10) 0.0138(10) 0.0164(10) 0.0031(8) 0.0010(8) 0.0000(8) C5 0.0133(10) 0.0148(10) 0.0158(10) 0.0048(8) -0.0003(8) -0.0015(8) C6 0.0155(10) 0.0167(10) 0.0167(10) 0.0061(8) 0.0008(8) -0.0014(8) N7 0.0122(8) 0.0118(8) 0.0153(8) 0.0034(7) -0.0009(7) 0.0005(7) C8 0.0150(10) 0.0150(10) 0.0176(10) 0.0043(8) -0.0017(8) 0.0001(8) N9 0.0165(9) 0.0132(8) 0.0186(9) 0.0048(7) -0.0029(7) 0.0014(7) C9 0.0216(12) 0.0172(11) 0.0279(12) 0.0079(9) -0.0036(9) 0.0040(9) N4 0.0133(9) 0.0148(9) 0.0262(10) 0.0057(7) 0.0038(7) 0.0005(7) N5 0.0197(9) 0.0164(9) 0.0144(9) 0.0029(7) 0.0019(7) 0.0015(7) C10 0.0324(14) 0.0296(13) 0.0193(11) 0.0022(10) 0.0084(10) 0.0073(11) C11 0.0215(12) 0.0271(12) 0.0325(13) 0.0116(10) 0.0136(10) 0.0047(10) C12 0.0170(11) 0.0240(11) 0.0148(10) 0.0025(9) 0.0036(8) 0.0033(9) C13 0.0205(11) 0.0226(11) 0.0146(10) -0.0013(9) -0.0007(8) 0.0038(9) C14 0.0194(11) 0.0239(11) 0.0188(11) 0.0100(9) -0.0029(9) -0.0007(9) C15 0.0219(11) 0.0162(10) 0.0229(11) 0.0088(9) -0.0030(9) 0.0013(9) C16 0.0162(11) 0.0209(11) 0.0224(11) 0.0042(9) 0.0003(9) -0.0069(9) C17 0.0125(10) 0.0231(11) 0.0212(11) 0.0008(9) -0.0015(8) -0.0060(9) P1 0.0180(3) 0.0210(3) 0.0228(3) 0.0049(2) 0.0025(2) 0.0006(2) P2 0.0195(4) 0.0340(5) 0.0233(4) 0.0156(4) -0.0060(3) -0.0045(4) P3 0.0222(4) 0.0210(4) 0.0175(4) -0.0019(3) 0.0000(3) 0.0003(3) F1 0.0231(7) 0.0541(9) 0.0314(8) 0.0018(7) 0.0045(6) 0.0108(7) F2 0.0458(10) 0.0507(10) 0.0615(11) 0.0254(9) 0.0336(9) 0.0263(8) F3 0.0374(9) 0.0399(8) 0.0356(8) 0.0203(7) 0.0008(7) 0.0027(7) F4 0.0306(8) 0.0455(9) 0.0343(8) 0.0226(7) -0.0036(6) -0.0011(7) F5 0.0309(8) 0.0275(8) 0.0705(12) 0.0082(8) -0.0238(8) -0.0066(7) F6 0.0579(11) 0.0284(8) 0.0399(9) 0.0017(7) -0.0120(8) -0.0104(7) F7 0.0202(7) 0.0503(9) 0.0346(8) 0.0220(7) -0.0068(6) -0.0071(7) F8 0.0375(9) 0.0686(12) 0.0395(9) -0.0081(8) -0.0056(7) 0.0022(8) F9 0.0290(8) 0.0601(11) 0.0632(11) 0.0464(9) -0.0065(8) -0.0041(8) F10 0.0427(10) 0.0494(10) 0.0417(9) -0.0081(8) -0.0083(8) -0.0187(8) F11 0.0471(10) 0.0448(9) 0.0418(9) 0.0013(8) 0.0071(8) 0.0233(8) F12 0.0570(11) 0.0440(9) 0.0271(8) 0.0129(7) 0.0063(7) 0.0025(8) O1w 0.0364(11) 0.0181(9) 0.0522(13) 0.0110(9) 0.0207(10) 0.0058(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N4 2.1422(17) . ? Ru N7 2.1549(16) . ? Ru N5 2.1609(17) . ? Ru S3 2.2852(5) . ? Ru S1 2.2934(5) . ? Ru S2 2.2993(5) . ? S1 C17 1.823(2) . ? S1 C12 1.834(2) . ? S3 C15 1.827(2) . ? S3 C16 1.843(2) . ? S2 C13 1.822(2) . ? S2 C14 1.841(2) . ? O1 C6 1.227(3) . ? N1 C2 1.368(3) . ? N1 C6 1.406(3) . ? N2 C2 1.339(3) . ? N3 C2 1.318(3) . ? N3 C4 1.357(3) . ? C5 C4 1.385(3) . ? C5 C6 1.427(3) . ? N7 C8 1.320(3) . ? N7 C5 1.400(3) . ? N9 C8 1.357(3) . ? N9 C4 1.366(3) . ? N9 C9 1.462(3) . ? N4 C11 1.483(3) . ? N5 C10 1.488(3) . ? C11 C10 1.507(3) . ? C12 C13 1.514(3) . ? C14 C15 1.517(3) . ? C17 C16 1.519(3) . ? P1 F6 1.5831(15) . ? P1 F1 1.5866(15) . ? P1 F3 1.5928(15) . ? P1 F2 1.5953(15) . ? P1 F4 1.6090(15) . ? P1 F5 1.6141(15) . ? P2 F8 1.5889(16) 2_565 ? P2 F8 1.5889(16) . ? P2 F9 1.5921(14) 2_565 ? P2 F9 1.5921(14) . ? P2 F7 1.6112(13) . ? P2 F7 1.6112(13) 2_565 ? P3 F11 1.5940(15) . ? P3 F11 1.5940(15) 2 ? P3 F12 1.5944(14) 2 ? P3 F12 1.5944(14) . ? P3 F10 1.5949(14) . ? P3 F10 1.5949(14) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ru N7 88.97(6) . . ? N4 Ru N5 80.28(7) . . ? N7 Ru N5 87.15(6) . . ? N4 Ru S3 91.72(5) . . ? N7 Ru S3 178.54(5) . . ? N5 Ru S3 91.69(5) . . ? N4 Ru S1 176.26(5) . . ? N7 Ru S1 90.48(5) . . ? N5 Ru S1 96.00(5) . . ? S3 Ru S1 88.753(19) . . ? N4 Ru S2 95.66(5) . . ? N7 Ru S2 92.58(5) . . ? N5 Ru S2 175.93(5) . . ? S3 Ru S2 88.636(19) . . ? S1 Ru S2 88.065(18) . . ? C17 S1 C12 101.02(10) . . ? C17 S1 Ru 103.73(7) . . ? C12 S1 Ru 106.41(7) . . ? C13 S2 C14 100.69(10) . . ? C13 S2 Ru 102.73(7) . . ? C14 S2 Ru 105.56(7) . . ? C15 S3 C16 100.64(10) . . ? C15 S3 Ru 103.07(7) . . ? C16 S3 Ru 106.26(7) . . ? C2 N1 C6 126.44(19) . . ? C2 N3 C4 112.63(18) . . ? N3 C2 N2 120.0(2) . . ? N3 C2 N1 123.1(2) . . ? N2 C2 N1 116.9(2) . . ? N3 C4 N9 124.84(19) . . ? N3 C4 C5 128.5(2) . . ? N9 C4 C5 106.67(17) . . ? C4 C5 N7 109.09(18) . . ? C4 C5 C6 118.79(18) . . ? N7 C5 C6 132.07(19) . . ? O1 C6 N1 119.05(19) . . ? O1 C6 C5 130.44(19) . . ? N1 C6 C5 110.50(18) . . ? C8 N7 C5 104.48(16) . . ? C8 N7 Ru 121.24(13) . . ? C5 N7 Ru 134.28(13) . . ? N7 C8 N9 113.17(18) . . ? C8 N9 C4 106.57(17) . . ? C8 N9 C9 126.34(18) . . ? C4 N9 C9 127.00(17) . . ? C11 N4 Ru 109.02(13) . . ? C10 N5 Ru 109.29(13) . . ? N5 C10 C11 108.67(18) . . ? N4 C11 C10 108.23(18) . . ? C13 C12 S1 110.94(14) . . ? C12 C13 S2 112.98(14) . . ? C15 C14 S2 110.58(15) . . ? C14 C15 S3 112.68(15) . . ? C17 C16 S3 112.42(15) . . ? C16 C17 S1 113.56(14) . . ? F6 P1 F1 90.29(9) . . ? F6 P1 F3 90.77(9) . . ? F1 P1 F3 90.06(8) . . ? F6 P1 F2 91.42(10) . . ? F1 P1 F2 178.14(10) . . ? F3 P1 F2 90.65(9) . . ? F6 P1 F4 90.06(8) . . ? F1 P1 F4 90.26(8) . . ? F3 P1 F4 179.11(9) . . ? F2 P1 F4 89.01(9) . . ? F6 P1 F5 179.35(9) . . ? F1 P1 F5 89.59(9) . . ? F3 P1 F5 89.87(9) . . ? F2 P1 F5 88.69(10) . . ? F4 P1 F5 89.30(9) . . ? F8 P2 F8 180.00(14) 2_565 . ? F8 P2 F9 89.71(10) 2_565 2_565 ? F8 P2 F9 90.29(10) . 2_565 ? F8 P2 F9 90.29(10) 2_565 . ? F8 P2 F9 89.71(10) . . ? F9 P2 F9 180.00(9) 2_565 . ? F8 P2 F7 89.82(8) 2_565 . ? F8 P2 F7 90.18(8) . . ? F9 P2 F7 90.59(7) 2_565 . ? F9 P2 F7 89.41(7) . . ? F8 P2 F7 90.18(8) 2_565 2_565 ? F8 P2 F7 89.82(8) . 2_565 ? F9 P2 F7 89.41(7) 2_565 2_565 ? F9 P2 F7 90.59(7) . 2_565 ? F7 P2 F7 180.0 . 2_565 ? F11 P3 F11 180.00(11) . 2 ? F11 P3 F12 90.68(8) . 2 ? F11 P3 F12 89.32(8) 2 2 ? F11 P3 F12 89.32(8) . . ? F11 P3 F12 90.68(8) 2 . ? F12 P3 F12 180.00(10) 2 . ? F11 P3 F10 89.91(9) . . ? F11 P3 F10 90.09(9) 2 . ? F12 P3 F10 90.28(9) 2 . ? F12 P3 F10 89.72(9) . . ? F11 P3 F10 90.09(9) . 2 ? F11 P3 F10 89.91(9) 2 2 ? F12 P3 F10 89.72(9) 2 2 ? F12 P3 F10 90.28(9) . 2 ? F10 P3 F10 180.00(16) . 2 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.409 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.080 #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 886392' #TrackingRef '- data2-4-10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H26 N6 O3 Ru S3 1+, (P F6 1-), 1.5(H2 O)' _chemical_formula_sum 'C18 H26 F6 N6 O4.50 P Ru S3' _chemical_formula_weight 740.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 '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 10.3000(10) _cell_length_b 14.2830(11) _cell_length_c 18.1920(14) _cell_angle_alpha 90.00 _cell_angle_beta 91.741(11) _cell_angle_gamma 90.00 _cell_volume 2675.1(4) _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 needle _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 8.272 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.2081 _exptl_absorpt_correction_T_max 0.3593 _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 1.54183 _diffrn_radiation_type CuK\a _diffrn_source 'Enraf Nonius FR590' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '135mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD2000 _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 14 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24838 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.94 _diffrn_reflns_theta_max 64.35 _reflns_number_total 4325 _reflns_number_gt 2995 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Supergui (Nonius BV, 1997-2000)' _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 1.80.05 (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^ > 2\s(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^)+(0.1070P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4325 _refine_ls_number_parameters 369 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1503 _refine_ls_wR_factor_gt 0.1421 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _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 0.05636(4) 0.44084(4) 0.28969(3) 0.0325(2) Uani 1 1 d . . . S3 S 0.00019(15) 0.59078(12) 0.26060(9) 0.0367(4) Uani 1 1 d . . . S2 S 0.07465(15) 0.48512(12) 0.40974(9) 0.0384(4) Uani 1 1 d . . . S1 S 0.27017(14) 0.48242(13) 0.27739(10) 0.0402(4) Uani 1 1 d . . . O1 O -0.0768(4) 0.2877(4) 0.4410(3) 0.0449(12) Uani 1 1 d . . . N1 N 0.0490(5) 0.1657(4) 0.4815(3) 0.0393(13) Uani 1 1 d . . . H1 H 0.0000 0.1603 0.5186 0.047 Uiso 1 1 calc R . . N2 N 0.1607(6) 0.0407(5) 0.5310(4) 0.0577(18) Uani 1 1 d . . . H2A H 0.2199 -0.0016 0.5294 0.069 Uiso 1 1 calc R . . H2B H 0.1099 0.0428 0.5676 0.069 Uiso 1 1 calc R . . C2 C 0.1475(7) 0.1030(6) 0.4767(4) 0.0469(18) Uani 1 1 d . . . N3 N 0.2262(5) 0.0997(4) 0.4199(3) 0.0444(14) Uani 1 1 d . . . C4 C 0.2031(6) 0.1714(5) 0.3729(4) 0.0405(16) Uani 1 1 d . . . C5 C 0.1103(6) 0.2420(5) 0.3745(4) 0.0354(15) Uani 1 1 d . . . C6 C 0.0195(6) 0.2375(5) 0.4328(4) 0.0380(16) Uani 1 1 d . . . N7 N 0.1220(5) 0.2999(4) 0.3136(3) 0.0348(12) Uani 1 1 d . . . C8 C 0.2189(6) 0.2629(5) 0.2765(4) 0.0393(16) Uani 1 1 d . . . H8 H 0.2479 0.2871 0.2325 0.047 Uiso 1 1 calc R . . N9 N 0.2704(5) 0.1869(4) 0.3096(3) 0.0422(14) Uani 1 1 d . . . C9 C 0.3713(8) 0.1260(6) 0.2817(5) 0.062(2) Uani 1 1 d . . . H9A H 0.4159 0.1576 0.2433 0.093 Uiso 1 1 calc R . . H9B H 0.3325 0.0696 0.2624 0.093 Uiso 1 1 calc R . . H9C H 0.4320 0.1105 0.3209 0.093 Uiso 1 1 calc R . . N4 N -0.1405(5) 0.4014(4) 0.2850(3) 0.0385(13) Uani 1 1 d . . . O2 O 0.0304(4) 0.4028(3) 0.1769(2) 0.0374(10) Uani 1 1 d . . . O3 O -0.1215(4) 0.3608(4) 0.0938(3) 0.0465(12) Uani 1 1 d . . . C10 C -0.0879(6) 0.3823(5) 0.1574(4) 0.0377(16) Uani 1 1 d . . . C11 C -0.1860(6) 0.3812(5) 0.2155(4) 0.0394(16) Uani 1 1 d . . . C12 C -0.3142(6) 0.3582(5) 0.2011(4) 0.0448(18) Uani 1 1 d . . . H12 H -0.3425 0.3440 0.1534 0.054 Uiso 1 1 calc R . . C13 C -0.4003(6) 0.3560(6) 0.2575(5) 0.054(2) Uani 1 1 d . . . H13 H -0.4872 0.3412 0.2484 0.065 Uiso 1 1 calc R . . C14 C -0.3545(6) 0.3764(5) 0.3279(4) 0.051(2) Uani 1 1 d . . . H14 H -0.4105 0.3746 0.3670 0.061 Uiso 1 1 calc R . . C15 C -0.2252(6) 0.3995(5) 0.3400(4) 0.0382(16) Uani 1 1 d . . . H15 H -0.1958 0.4141 0.3874 0.046 Uiso 1 1 calc R . . C16 C 0.0115(7) 0.6568(5) 0.3472(4) 0.0456(18) Uani 1 1 d . . . H16A H 0.0979 0.6834 0.3531 0.055 Uiso 1 1 calc R . . H16B H -0.0503 0.7081 0.3451 0.055 Uiso 1 1 calc R . . C17 C -0.0153(7) 0.5967(5) 0.4123(4) 0.0477(18) Uani 1 1 d . . . H17A H -0.1077 0.5837 0.4134 0.057 Uiso 1 1 calc R . . H17B H 0.0092 0.6302 0.4570 0.057 Uiso 1 1 calc R . . C18 C 0.2429(6) 0.5297(6) 0.4250(4) 0.0461(18) Uani 1 1 d . . . H18A H 0.2439 0.5970 0.4182 0.055 Uiso 1 1 calc R . . H18B H 0.2721 0.5163 0.4751 0.055 Uiso 1 1 calc R . . C19 C 0.3336(6) 0.4846(6) 0.3722(4) 0.0475(18) Uani 1 1 d . . . H19A H 0.3509 0.4208 0.3881 0.057 Uiso 1 1 calc R . . H19B H 0.4154 0.5182 0.3739 0.057 Uiso 1 1 calc R . . C20 C 0.2700(6) 0.6078(5) 0.2534(4) 0.0448(18) Uani 1 1 d . . . H20A H 0.2810 0.6450 0.2978 0.054 Uiso 1 1 calc R . . H20B H 0.3419 0.6212 0.2219 0.054 Uiso 1 1 calc R . . C21 C 0.1426(6) 0.6336(5) 0.2140(4) 0.0425(17) Uani 1 1 d . . . H21A H 0.1422 0.6080 0.1646 0.051 Uiso 1 1 calc R . . H21B H 0.1371 0.7012 0.2099 0.051 Uiso 1 1 calc R . . P1 P 0.41109(18) 0.19338(16) 0.05746(11) 0.0511(5) Uani 1 1 d . . . F1 F 0.5056(6) 0.1396(5) 0.0061(3) 0.108(2) Uani 1 1 d . . . F2 F 0.2973(5) 0.1871(5) -0.0036(3) 0.099(2) Uani 1 1 d . . . F3 F 0.3130(6) 0.2414(5) 0.1103(3) 0.100(2) Uani 1 1 d . . . F4 F 0.5210(5) 0.1943(4) 0.1209(3) 0.0826(16) Uani 1 1 d . . . F5 F 0.4560(6) 0.2918(4) 0.0291(4) 0.105(2) Uani 1 1 d . . . F6 F 0.3661(5) 0.0934(4) 0.0875(3) 0.0936(18) Uani 1 1 d . . . O1W O 0.3069(8) 0.6425(8) 0.0650(5) 0.110(3) Uani 1 1 d D . . H1W H 0.342(15) 0.699(5) 0.054(8) 0.165 Uiso 1 1 d D . . H2W H 0.377(10) 0.607(9) 0.054(8) 0.165 Uiso 1 1 d D . . O2W O 0.5274(14) 0.5084(12) 0.0713(10) 0.119(6) 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 0.0252(3) 0.0350(3) 0.0367(3) -0.0005(2) -0.00547(18) -0.0003(2) S3 0.0328(8) 0.0353(10) 0.0415(10) 0.0038(7) -0.0065(6) 0.0020(7) S2 0.0392(8) 0.0387(10) 0.0368(9) -0.0017(8) -0.0071(6) 0.0016(7) S1 0.0270(7) 0.0429(10) 0.0505(10) 0.0054(8) -0.0049(6) -0.0018(7) O1 0.037(2) 0.049(3) 0.049(3) 0.003(2) -0.001(2) 0.004(2) N1 0.037(3) 0.044(4) 0.037(3) 0.006(3) 0.002(2) 0.001(3) N2 0.061(4) 0.051(4) 0.061(4) 0.019(3) 0.005(3) 0.017(3) C2 0.046(4) 0.048(5) 0.047(5) 0.002(4) -0.005(3) 0.001(3) N3 0.039(3) 0.042(4) 0.052(4) 0.004(3) -0.001(3) 0.005(3) C4 0.036(3) 0.044(4) 0.041(4) -0.005(3) -0.007(3) -0.001(3) C5 0.032(3) 0.031(4) 0.042(4) 0.000(3) -0.006(3) 0.000(3) C6 0.033(3) 0.042(4) 0.039(4) -0.001(3) -0.009(3) -0.008(3) N7 0.035(3) 0.028(3) 0.041(3) 0.002(3) -0.004(2) 0.005(2) C8 0.034(3) 0.041(4) 0.042(4) 0.004(3) -0.005(3) -0.002(3) N9 0.030(3) 0.044(4) 0.052(4) 0.000(3) -0.001(2) -0.004(2) C9 0.055(5) 0.048(5) 0.085(6) 0.005(5) 0.018(4) 0.018(4) N4 0.026(3) 0.033(3) 0.056(4) 0.002(3) -0.008(2) 0.002(2) O2 0.035(2) 0.043(3) 0.034(2) -0.005(2) -0.0029(17) -0.001(2) O3 0.041(3) 0.056(3) 0.042(3) -0.007(2) -0.007(2) 0.006(2) C10 0.039(4) 0.042(4) 0.032(4) 0.003(3) -0.002(3) -0.002(3) C11 0.033(3) 0.047(5) 0.037(4) -0.002(3) -0.008(3) 0.001(3) C12 0.032(3) 0.044(5) 0.057(5) -0.009(4) -0.009(3) -0.005(3) C13 0.025(3) 0.061(5) 0.076(6) -0.009(4) -0.002(3) 0.000(3) C14 0.034(4) 0.050(5) 0.070(5) 0.006(4) 0.012(3) 0.002(3) C15 0.029(3) 0.044(4) 0.041(4) 0.006(3) 0.002(3) 0.003(3) C16 0.050(4) 0.033(4) 0.054(5) -0.009(4) 0.000(3) 0.011(3) C17 0.051(4) 0.044(4) 0.047(4) -0.008(4) -0.004(3) 0.001(3) C18 0.045(4) 0.045(5) 0.047(4) -0.004(4) -0.014(3) -0.003(3) C19 0.027(3) 0.053(5) 0.061(5) 0.004(4) -0.019(3) -0.002(3) C20 0.033(3) 0.040(4) 0.061(5) 0.004(4) -0.003(3) -0.009(3) C21 0.036(3) 0.043(4) 0.048(4) 0.010(3) -0.004(3) -0.005(3) P1 0.0430(10) 0.0593(14) 0.0503(12) -0.0020(10) -0.0108(8) 0.0085(9) F1 0.095(4) 0.157(6) 0.072(4) -0.011(4) 0.003(3) 0.061(4) F2 0.088(4) 0.106(5) 0.101(4) -0.010(4) -0.053(3) 0.032(3) F3 0.089(4) 0.124(5) 0.088(4) -0.012(4) 0.014(3) 0.032(4) F4 0.069(3) 0.083(4) 0.093(4) 0.000(3) -0.044(3) -0.007(3) F5 0.091(4) 0.088(4) 0.135(5) 0.048(4) 0.001(4) -0.006(3) F6 0.077(4) 0.075(4) 0.126(5) 0.025(4) -0.032(3) -0.018(3) O1W 0.080(5) 0.146(8) 0.104(6) 0.005(6) 0.015(4) -0.008(5) O2W 0.068(9) 0.119(14) 0.169(16) -0.012(13) -0.005(9) -0.036(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N4 2.104(5) . ? Ru O2 2.132(4) . ? Ru N7 2.164(5) . ? Ru S2 2.2760(17) . ? Ru S3 2.2765(17) . ? Ru S1 2.2984(16) . ? S3 C21 1.821(6) . ? S3 C16 1.837(7) . ? S2 C17 1.844(8) . ? S2 C18 1.859(7) . ? S1 C19 1.826(7) . ? S1 C20 1.842(7) . ? O1 C6 1.238(8) . ? N1 C2 1.358(9) . ? N1 C6 1.382(8) . ? N1 H1 0.8600 . ? N2 C2 1.334(9) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? C2 N3 1.332(9) . ? N3 C4 1.350(9) . ? C4 N9 1.380(8) . ? C4 C5 1.390(9) . ? C5 N7 1.390(8) . ? C5 C6 1.437(9) . ? N7 C8 1.331(8) . ? C8 N9 1.343(9) . ? C8 H8 0.9300 . ? N9 C9 1.459(9) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? N4 C15 1.346(8) . ? N4 C11 1.367(8) . ? O2 C10 1.291(8) . ? O3 C10 1.238(8) . ? C10 C11 1.484(9) . ? C11 C12 1.378(9) . ? C12 C13 1.376(10) . ? C12 H12 0.9300 . ? C13 C14 1.382(11) . ? C13 H13 0.9300 . ? C14 C15 1.384(10) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.495(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.505(10) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.522(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? P1 F1 1.570(5) . ? P1 F5 1.572(6) . ? P1 F3 1.573(5) . ? P1 F4 1.592(5) . ? P1 F2 1.592(5) . ? P1 F6 1.602(6) . ? O1W H1W 0.91(2) . ? O1W H2W 0.90(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ru O2 78.48(19) . . ? N4 Ru N7 93.1(2) . . ? O2 Ru N7 89.16(19) . . ? N4 Ru S2 99.47(16) . . ? O2 Ru S2 177.22(12) . . ? N7 Ru S2 92.83(15) . . ? N4 Ru S3 90.27(15) . . ? O2 Ru S3 89.58(13) . . ? N7 Ru S3 176.11(14) . . ? S2 Ru S3 88.55(6) . . ? N4 Ru S1 172.10(16) . . ? O2 Ru S1 93.73(12) . . ? N7 Ru S1 88.02(14) . . ? S2 Ru S1 88.28(6) . . ? S3 Ru S1 88.38(6) . . ? C21 S3 C16 101.3(3) . . ? C21 S3 Ru 102.8(2) . . ? C16 S3 Ru 105.9(2) . . ? C17 S2 C18 99.6(3) . . ? C17 S2 Ru 103.7(2) . . ? C18 S2 Ru 106.7(2) . . ? C19 S1 C20 101.8(4) . . ? C19 S1 Ru 103.2(2) . . ? C20 S1 Ru 106.3(2) . . ? C2 N1 C6 126.7(6) . . ? C2 N1 H1 116.6 . . ? C6 N1 H1 116.6 . . ? C2 N2 H2A 120.0 . . ? C2 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? N3 C2 N2 120.0(7) . . ? N3 C2 N1 123.1(7) . . ? N2 C2 N1 116.9(6) . . ? C2 N3 C4 111.4(6) . . ? N3 C4 N9 124.5(6) . . ? N3 C4 C5 130.2(6) . . ? N9 C4 C5 105.3(6) . . ? C4 C5 N7 109.8(6) . . ? C4 C5 C6 116.4(6) . . ? N7 C5 C6 133.6(6) . . ? O1 C6 N1 120.9(6) . . ? O1 C6 C5 127.2(6) . . ? N1 C6 C5 111.8(6) . . ? C8 N7 C5 104.6(5) . . ? C8 N7 Ru 120.1(4) . . ? C5 N7 Ru 132.8(4) . . ? N7 C8 N9 112.7(6) . . ? N7 C8 H8 123.6 . . ? N9 C8 H8 123.6 . . ? C8 N9 C4 107.6(6) . . ? C8 N9 C9 127.0(6) . . ? C4 N9 C9 125.2(6) . . ? N9 C9 H9A 109.5 . . ? N9 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N9 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 N4 C11 118.1(5) . . ? C15 N4 Ru 128.4(5) . . ? C11 N4 Ru 113.4(4) . . ? C10 O2 Ru 114.3(4) . . ? O3 C10 O2 123.2(6) . . ? O3 C10 C11 119.1(6) . . ? O2 C10 C11 117.7(6) . . ? N4 C11 C12 121.7(6) . . ? N4 C11 C10 115.8(5) . . ? C12 C11 C10 122.5(6) . . ? C13 C12 C11 120.0(7) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 118.4(6) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C13 C14 C15 119.8(6) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? N4 C15 C14 121.9(7) . . ? N4 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C17 C16 S3 112.1(5) . . ? C17 C16 H16A 109.2 . . ? S3 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? S3 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 S2 111.8(5) . . ? C16 C17 H17A 109.3 . . ? S2 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? S2 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? C19 C18 S2 110.6(5) . . ? C19 C18 H18A 109.5 . . ? S2 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? S2 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C18 C19 S1 113.5(5) . . ? C18 C19 H19A 108.9 . . ? S1 C19 H19A 108.9 . . ? C18 C19 H19B 108.9 . . ? S1 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? C21 C20 S1 110.0(5) . . ? C21 C20 H20A 109.7 . . ? S1 C20 H20A 109.7 . . ? C21 C20 H20B 109.7 . . ? S1 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C20 C21 S3 113.3(5) . . ? C20 C21 H21A 108.9 . . ? S3 C21 H21A 108.9 . . ? C20 C21 H21B 108.9 . . ? S3 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? F1 P1 F5 92.8(4) . . ? F1 P1 F3 176.5(4) . . ? F5 P1 F3 90.7(4) . . ? F1 P1 F4 89.7(3) . . ? F5 P1 F4 91.2(3) . . ? F3 P1 F4 90.5(3) . . ? F1 P1 F2 90.8(3) . . ? F5 P1 F2 92.2(4) . . ? F3 P1 F2 88.8(3) . . ? F4 P1 F2 176.5(4) . . ? F1 P1 F6 87.5(4) . . ? F5 P1 F6 179.2(4) . . ? F3 P1 F6 89.0(4) . . ? F4 P1 F6 88.1(3) . . ? F2 P1 F6 88.5(3) . . ? H1W O1W H2W 97(10) . . ? 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 N4 Ru S3 C21 -151.7(3) . . . . ? O2 Ru S3 C21 -73.2(3) . . . . ? N7 Ru S3 C21 -2(2) . . . . ? S2 Ru S3 C21 108.8(2) . . . . ? S1 Ru S3 C21 20.5(2) . . . . ? N4 Ru S3 C16 102.4(3) . . . . ? O2 Ru S3 C16 -179.1(3) . . . . ? N7 Ru S3 C16 -108(2) . . . . ? S2 Ru S3 C16 2.9(2) . . . . ? S1 Ru S3 C16 -85.4(2) . . . . ? N4 Ru S2 C17 -72.3(3) . . . . ? O2 Ru S2 C17 -30(3) . . . . ? N7 Ru S2 C17 -165.9(3) . . . . ? S3 Ru S2 C17 17.7(2) . . . . ? S1 Ru S2 C17 106.1(3) . . . . ? N4 Ru S2 C18 -177.0(3) . . . . ? O2 Ru S2 C18 -135(3) . . . . ? N7 Ru S2 C18 89.4(3) . . . . ? S3 Ru S2 C18 -87.0(3) . . . . ? S1 Ru S2 C18 1.5(3) . . . . ? N4 Ru S1 C19 -172.3(11) . . . . ? O2 Ru S1 C19 -163.1(3) . . . . ? N7 Ru S1 C19 -74.1(3) . . . . ? S2 Ru S1 C19 18.8(3) . . . . ? S3 Ru S1 C19 107.4(3) . . . . ? N4 Ru S1 C20 81.0(12) . . . . ? O2 Ru S1 C20 90.2(3) . . . . ? N7 Ru S1 C20 179.2(3) . . . . ? S2 Ru S1 C20 -87.9(3) . . . . ? S3 Ru S1 C20 0.7(3) . . . . ? C6 N1 C2 N3 -4.1(11) . . . . ? C6 N1 C2 N2 178.3(6) . . . . ? N2 C2 N3 C4 -176.4(7) . . . . ? N1 C2 N3 C4 6.0(10) . . . . ? C2 N3 C4 N9 179.2(7) . . . . ? C2 N3 C4 C5 -2.5(10) . . . . ? N3 C4 C5 N7 -179.1(6) . . . . ? N9 C4 C5 N7 -0.6(7) . . . . ? N3 C4 C5 C6 -3.3(11) . . . . ? N9 C4 C5 C6 175.3(5) . . . . ? C2 N1 C6 O1 176.5(6) . . . . ? C2 N1 C6 C5 -2.1(9) . . . . ? C4 C5 C6 O1 -173.3(7) . . . . ? N7 C5 C6 O1 1.3(12) . . . . ? C4 C5 C6 N1 5.1(8) . . . . ? N7 C5 C6 N1 179.8(6) . . . . ? C4 C5 N7 C8 0.8(7) . . . . ? C6 C5 N7 C8 -174.1(7) . . . . ? C4 C5 N7 Ru -160.7(4) . . . . ? C6 C5 N7 Ru 24.4(11) . . . . ? N4 Ru N7 C8 132.5(5) . . . . ? O2 Ru N7 C8 54.1(5) . . . . ? S2 Ru N7 C8 -127.9(5) . . . . ? S3 Ru N7 C8 -17(2) . . . . ? S1 Ru N7 C8 -39.7(5) . . . . ? N4 Ru N7 C5 -68.3(6) . . . . ? O2 Ru N7 C5 -146.8(5) . . . . ? S2 Ru N7 C5 31.3(5) . . . . ? S3 Ru N7 C5 142.0(19) . . . . ? S1 Ru N7 C5 119.5(5) . . . . ? C5 N7 C8 N9 -0.7(7) . . . . ? Ru N7 C8 N9 163.7(4) . . . . ? N7 C8 N9 C4 0.4(8) . . . . ? N7 C8 N9 C9 175.5(7) . . . . ? N3 C4 N9 C8 178.8(6) . . . . ? C5 C4 N9 C8 0.2(7) . . . . ? N3 C4 N9 C9 3.5(11) . . . . ? C5 C4 N9 C9 -175.1(7) . . . . ? O2 Ru N4 C15 178.8(6) . . . . ? N7 Ru N4 C15 90.3(6) . . . . ? S2 Ru N4 C15 -3.1(6) . . . . ? S3 Ru N4 C15 -91.7(6) . . . . ? S1 Ru N4 C15 -171.8(8) . . . . ? O2 Ru N4 C11 -5.5(5) . . . . ? N7 Ru N4 C11 -94.0(5) . . . . ? S2 Ru N4 C11 172.6(4) . . . . ? S3 Ru N4 C11 84.0(5) . . . . ? S1 Ru N4 C11 3.9(15) . . . . ? N4 Ru O2 C10 5.3(5) . . . . ? N7 Ru O2 C10 98.7(5) . . . . ? S2 Ru O2 C10 -37(3) . . . . ? S3 Ru O2 C10 -85.0(5) . . . . ? S1 Ru O2 C10 -173.4(4) . . . . ? Ru O2 C10 O3 178.3(5) . . . . ? Ru O2 C10 C11 -4.2(8) . . . . ? C15 N4 C11 C12 -0.9(10) . . . . ? Ru N4 C11 C12 -177.0(6) . . . . ? C15 N4 C11 C10 -178.7(6) . . . . ? Ru N4 C11 C10 5.2(8) . . . . ? O3 C10 C11 N4 177.0(6) . . . . ? O2 C10 C11 N4 -0.6(10) . . . . ? O3 C10 C11 C12 -0.8(11) . . . . ? O2 C10 C11 C12 -178.4(7) . . . . ? N4 C11 C12 C13 0.7(12) . . . . ? C10 C11 C12 C13 178.4(7) . . . . ? C11 C12 C13 C14 -0.7(12) . . . . ? C12 C13 C14 C15 0.9(12) . . . . ? C11 N4 C15 C14 1.1(10) . . . . ? Ru N4 C15 C14 176.6(5) . . . . ? C13 C14 C15 N4 -1.1(11) . . . . ? C21 S3 C16 C17 -136.4(5) . . . . ? Ru S3 C16 C17 -29.4(5) . . . . ? S3 C16 C17 S2 47.1(6) . . . . ? C18 S2 C17 C16 68.6(6) . . . . ? Ru S2 C17 C16 -41.4(6) . . . . ? C17 S2 C18 C19 -134.7(5) . . . . ? Ru S2 C18 C19 -27.1(6) . . . . ? S2 C18 C19 S1 46.4(7) . . . . ? C20 S1 C19 C18 67.5(6) . . . . ? Ru S1 C19 C18 -42.5(6) . . . . ? C19 S1 C20 C21 -134.9(5) . . . . ? Ru S1 C20 C21 -27.2(5) . . . . ? S1 C20 C21 S3 48.2(7) . . . . ? C16 S3 C21 C20 64.5(6) . . . . ? Ru S3 C21 C20 -45.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 64.35 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.056 _refine_diff_density_min -1.530 _refine_diff_density_rms 0.155