# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Alessio, Enzo' _publ_contact_author_name 'Alessio, Enzo' _publ_contact_author_email alessi@units.it _publ_section_title ; New half sandwich-type Ru(II) coordination compounds characterized by the fac-Ru(dmso-S)3 fragment: influence of the face-capping group on the chemical behavior and in vitro anticancer activity ; # Attachment '- Alessio- Bratsos CIF files.txt' data_2P-BF4 _database_code_depnum_ccdc_archive 'CCDC 828778' #TrackingRef '- Alessio- Bratsos CIF files.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H30 B Cl F4 O5 Ru S5' _chemical_formula_weight 613.97 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' 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' Cl Cl 0.1484 0.1585 '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' B B 0.0013 0.0007 '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' _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 10.9250(11) _cell_length_b 18.0620(17) _cell_length_c 12.0490(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.175(11) _cell_angle_gamma 90.00 _cell_volume 2377.1(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 rectangular-prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 1.260 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7183 _exptl_absorpt_correction_T_max 0.7531 _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 6594 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 29.64 _reflns_number_total 6594 _reflns_number_gt 4612 _reflns_threshold_expression >2\s(I) _computing_data_collection 'XPRESS (MacScience, 2002)' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX97 (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^)+(0.0455P)^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 6594 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.927 _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 0.233664(17) 0.161408(12) 0.346552(16) 0.04358(7) Uani 1 1 d . . . Cl1 Cl 0.22190(6) 0.03013(4) 0.38325(6) 0.05852(17) Uani 1 1 d . . . S1 S 0.36233(6) 0.15162(4) 0.20360(6) 0.05104(16) Uani 1 1 d . . . S2 S 0.05819(6) 0.15426(4) 0.24648(6) 0.05254(16) Uani 1 1 d . . . S3 S 0.24193(6) 0.28731(4) 0.33300(6) 0.05054(16) Uani 1 1 d . . . S4 S 0.17106(6) 0.13442(4) 0.59976(6) 0.05379(17) Uani 1 1 d . . . S5 S 0.48550(6) 0.10818(4) 0.47090(6) 0.05582(18) Uani 1 1 d . . . O1 O 0.48053(17) 0.18867(14) 0.22796(18) 0.0701(6) Uani 1 1 d . . . O2 O 0.01961(18) 0.21787(12) 0.17807(18) 0.0691(6) Uani 1 1 d . . . O3 O 0.2553(2) 0.32187(11) 0.22338(17) 0.0626(5) Uani 1 1 d . . . O4 O 0.13190(16) 0.17791(11) 0.49438(15) 0.0543(5) Uani 1 1 d . . . O5 O 0.38504(16) 0.16724(10) 0.46168(15) 0.0510(4) Uani 1 1 d . . . C1 C 0.3102(3) 0.1869(2) 0.0731(2) 0.0645(8) Uani 1 1 d . . . H1A H 0.2933 0.2389 0.0799 0.097 Uiso 1 1 calc R . . H1B H 0.2369 0.1614 0.0501 0.097 Uiso 1 1 calc R . . H1C H 0.3723 0.1796 0.0190 0.097 Uiso 1 1 calc R . . C2 C 0.3981(3) 0.05945(18) 0.1658(3) 0.0719(9) Uani 1 1 d . . . H2A H 0.4504 0.0599 0.1028 0.108 Uiso 1 1 calc R . . H2B H 0.3239 0.0333 0.1472 0.108 Uiso 1 1 calc R . . H2C H 0.4392 0.0352 0.2269 0.108 Uiso 1 1 calc R . . C3 C 0.0466(3) 0.07436(19) 0.1600(3) 0.0674(8) Uani 1 1 d . . . H3A H -0.0368 0.0682 0.1350 0.101 Uiso 1 1 calc R . . H3B H 0.0722 0.0315 0.2014 0.101 Uiso 1 1 calc R . . H3C H 0.0981 0.0804 0.0971 0.101 Uiso 1 1 calc R . . C4 C -0.0655(3) 0.1345(2) 0.3368(3) 0.0748(9) Uani 1 1 d . . . H4A H -0.0711 0.1730 0.3915 0.112 Uiso 1 1 calc R . . H4B H -0.0512 0.0879 0.3731 0.112 Uiso 1 1 calc R . . H4C H -0.1407 0.1322 0.2943 0.112 Uiso 1 1 calc R . . C5 C 0.1132(3) 0.32965(17) 0.3958(3) 0.0696(9) Uani 1 1 d . . . H5A H 0.1232 0.3825 0.3954 0.104 Uiso 1 1 calc R . . H5B H 0.1071 0.3126 0.4709 0.104 Uiso 1 1 calc R . . H5C H 0.0400 0.3167 0.3548 0.104 Uiso 1 1 calc R . . C6 C 0.3614(3) 0.32360(18) 0.4190(3) 0.0708(9) Uani 1 1 d . . . H6A H 0.4390 0.3073 0.3922 0.106 Uiso 1 1 calc R . . H6B H 0.3515 0.3065 0.4937 0.106 Uiso 1 1 calc R . . H6C H 0.3582 0.3767 0.4177 0.106 Uiso 1 1 calc R . . C7 C 0.0268(3) 0.1104(2) 0.6552(3) 0.0792(10) Uani 1 1 d . . . H7A H -0.0228 0.1540 0.6610 0.119 Uiso 1 1 calc R . . H7B H 0.0389 0.0888 0.7274 0.119 Uiso 1 1 calc R . . H7C H -0.0135 0.0753 0.6070 0.119 Uiso 1 1 calc R . . C8 C 0.2172(3) 0.20399(19) 0.6961(3) 0.0688(8) Uani 1 1 d . . . H8A H 0.2934 0.2251 0.6737 0.103 Uiso 1 1 calc R . . H8B H 0.2272 0.1825 0.7686 0.103 Uiso 1 1 calc R . . H8C H 0.1559 0.2420 0.6981 0.103 Uiso 1 1 calc R . . C9 C 0.4930(3) 0.0888(2) 0.6143(3) 0.0712(9) Uani 1 1 d . . . H9A H 0.4887 0.1342 0.6554 0.107 Uiso 1 1 calc R . . H9B H 0.5687 0.0641 0.6321 0.107 Uiso 1 1 calc R . . H9C H 0.4256 0.0575 0.6335 0.107 Uiso 1 1 calc R . . C10 C 0.6235(3) 0.1597(2) 0.4646(3) 0.0915(13) Uani 1 1 d . . . H10A H 0.6344 0.1771 0.3901 0.137 Uiso 1 1 calc R . . H10B H 0.6913 0.1287 0.4861 0.137 Uiso 1 1 calc R . . H10C H 0.6194 0.2013 0.5140 0.137 Uiso 1 1 calc R . . B1 B 0.7714(4) 0.4811(3) 0.3697(3) 0.0733(10) Uani 1 1 d . . . F1 F 0.6721(2) 0.43735(18) 0.3989(2) 0.1241(9) Uani 1 1 d . . . F2 F 0.7507(3) 0.50431(17) 0.26494(19) 0.1191(9) Uani 1 1 d . . . F3 F 0.7771(3) 0.53665(19) 0.4412(3) 0.1648(14) Uani 1 1 d . . . F4 F 0.87452(19) 0.43917(14) 0.3764(2) 0.1062(8) 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 0.03964(10) 0.04390(13) 0.04722(12) -0.00015(9) 0.00178(8) 0.00021(8) Cl1 0.0574(4) 0.0447(4) 0.0734(4) 0.0034(3) 0.0007(3) -0.0013(3) S1 0.0463(3) 0.0561(4) 0.0508(3) -0.0010(3) 0.0059(3) 0.0019(3) S2 0.0425(3) 0.0573(4) 0.0577(4) -0.0010(3) -0.0030(3) -0.0015(3) S3 0.0517(3) 0.0446(4) 0.0553(4) 0.0011(3) 0.0008(3) 0.0005(3) S4 0.0503(3) 0.0593(4) 0.0519(4) 0.0044(3) 0.0060(3) 0.0047(3) S5 0.0450(3) 0.0618(5) 0.0605(4) -0.0067(4) -0.0025(3) 0.0062(3) O1 0.0488(10) 0.0889(16) 0.0728(13) -0.0021(12) 0.0089(9) -0.0107(10) O2 0.0615(12) 0.0696(15) 0.0755(14) 0.0108(11) -0.0186(10) 0.0042(10) O3 0.0732(12) 0.0547(12) 0.0600(11) 0.0122(9) 0.0025(10) -0.0018(10) O4 0.0538(10) 0.0598(12) 0.0494(10) 0.0048(9) 0.0067(8) 0.0114(9) O5 0.0479(9) 0.0498(11) 0.0551(10) -0.0009(8) -0.0068(8) 0.0032(8) C1 0.0685(18) 0.071(2) 0.0546(16) 0.0089(15) 0.0073(14) 0.0068(16) C2 0.084(2) 0.069(2) 0.0633(18) -0.0030(16) 0.0153(16) 0.0232(18) C3 0.0660(17) 0.068(2) 0.0679(18) -0.0121(16) -0.0087(14) -0.0066(16) C4 0.0444(14) 0.100(3) 0.080(2) -0.006(2) 0.0038(14) -0.0114(16) C5 0.0717(19) 0.0535(19) 0.084(2) -0.0009(16) 0.0103(17) 0.0153(15) C6 0.079(2) 0.0531(19) 0.080(2) -0.0043(16) -0.0104(17) -0.0115(16) C7 0.0647(19) 0.098(3) 0.075(2) 0.024(2) 0.0130(16) -0.0069(18) C8 0.0702(18) 0.074(2) 0.0625(18) -0.0032(16) -0.0012(15) 0.0033(16) C9 0.0653(18) 0.076(2) 0.0724(19) 0.0157(17) -0.0001(15) 0.0152(16) C10 0.0468(16) 0.129(4) 0.098(3) 0.025(2) 0.0030(17) -0.0068(19) B1 0.067(2) 0.086(3) 0.067(2) 0.000(2) -0.0011(18) 0.015(2) F1 0.0845(15) 0.161(3) 0.127(2) 0.0286(18) 0.0086(13) -0.0065(16) F2 0.1329(19) 0.144(2) 0.0800(14) 0.0243(15) -0.0021(14) 0.0351(17) F3 0.194(3) 0.146(3) 0.154(3) -0.089(2) -0.030(2) 0.032(2) F4 0.0782(13) 0.123(2) 0.1179(17) 0.0283(15) 0.0115(12) 0.0305(13) _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 O5 2.1393(17) . ? Ru O4 2.1398(17) . ? Ru S2 2.2474(7) . ? Ru S1 2.2524(7) . ? Ru S3 2.2818(8) . ? Ru Cl1 2.4159(8) . ? S1 O1 1.478(2) . ? S1 C2 1.772(3) . ? S1 C1 1.779(3) . ? S2 O2 1.471(2) . ? S2 C3 1.783(3) . ? S2 C4 1.789(3) . ? S3 O3 1.471(2) . ? S3 C6 1.775(3) . ? S3 C5 1.783(3) . ? S4 O4 1.5460(19) . ? S4 C8 1.777(3) . ? S4 C7 1.778(3) . ? S5 O5 1.5329(19) . ? S5 C9 1.763(3) . ? S5 C10 1.775(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? B1 F3 1.324(5) . ? B1 F2 1.345(4) . ? B1 F4 1.358(4) . ? B1 F1 1.393(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Ru O4 82.03(7) . . ? O5 Ru S2 172.02(5) . . ? O4 Ru S2 90.14(5) . . ? O5 Ru S1 90.77(5) . . ? O4 Ru S1 172.11(5) . . ? S2 Ru S1 97.13(3) . . ? O5 Ru S3 88.06(5) . . ? O4 Ru S3 86.72(6) . . ? S2 Ru S3 93.06(3) . . ? S1 Ru S3 89.84(3) . . ? O5 Ru Cl1 88.45(5) . . ? O4 Ru Cl1 87.35(6) . . ? S2 Ru Cl1 89.64(3) . . ? S1 Ru Cl1 95.70(3) . . ? S3 Ru Cl1 173.49(3) . . ? O1 S1 C2 106.28(15) . . ? O1 S1 C1 106.00(14) . . ? C2 S1 C1 100.23(16) . . ? O1 S1 Ru 111.65(9) . . ? C2 S1 Ru 114.50(11) . . ? C1 S1 Ru 117.01(10) . . ? O2 S2 C3 106.78(15) . . ? O2 S2 C4 106.57(16) . . ? C3 S2 C4 98.58(16) . . ? O2 S2 Ru 119.16(9) . . ? C3 S2 Ru 114.18(11) . . ? C4 S2 Ru 109.38(11) . . ? O3 S3 C6 106.41(15) . . ? O3 S3 C5 107.00(15) . . ? C6 S3 C5 99.82(17) . . ? O3 S3 Ru 119.48(9) . . ? C6 S3 Ru 110.85(11) . . ? C5 S3 Ru 111.37(11) . . ? O4 S4 C8 104.32(14) . . ? O4 S4 C7 101.53(14) . . ? C8 S4 C7 99.74(17) . . ? O5 S5 C9 103.18(13) . . ? O5 S5 C10 103.84(16) . . ? C9 S5 C10 97.13(18) . . ? S4 O4 Ru 118.24(10) . . ? S5 O5 Ru 123.75(11) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S1 C2 H2A 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? S1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? S2 C3 H3A 109.5 . . ? S2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? S2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? S2 C4 H4A 109.5 . . ? S2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? S3 C5 H5A 109.5 . . ? S3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? S3 C6 H6A 109.5 . . ? S3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? S3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? S4 C7 H7A 109.5 . . ? S4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? S4 C8 H8A 109.5 . . ? S4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? S5 C9 H9A 109.5 . . ? S5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? S5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? S5 C10 H10A 109.5 . . ? S5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? S5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? F3 B1 F2 112.3(4) . . ? F3 B1 F4 110.8(4) . . ? F2 B1 F4 110.7(3) . . ? F3 B1 F1 106.9(3) . . ? F2 B1 F1 107.3(3) . . ? F4 B1 F1 108.5(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 O5 Ru S1 O1 -28.54(12) . . . . ? O4 Ru S1 O1 -4.6(4) . . . . ? S2 Ru S1 O1 152.59(11) . . . . ? S3 Ru S1 O1 59.52(11) . . . . ? Cl1 Ru S1 O1 -117.06(11) . . . . ? O5 Ru S1 C2 92.27(14) . . . . ? O4 Ru S1 C2 116.3(4) . . . . ? S2 Ru S1 C2 -86.60(13) . . . . ? S3 Ru S1 C2 -179.67(13) . . . . ? Cl1 Ru S1 C2 3.75(13) . . . . ? O5 Ru S1 C1 -150.89(14) . . . . ? O4 Ru S1 C1 -126.9(4) . . . . ? S2 Ru S1 C1 30.23(14) . . . . ? S3 Ru S1 C1 -62.84(14) . . . . ? Cl1 Ru S1 C1 120.58(14) . . . . ? O5 Ru S2 O2 115.0(4) . . . . ? O4 Ru S2 O2 103.83(12) . . . . ? S1 Ru S2 O2 -73.11(11) . . . . ? S3 Ru S2 O2 17.11(11) . . . . ? Cl1 Ru S2 O2 -168.82(11) . . . . ? O5 Ru S2 C3 -117.2(4) . . . . ? O4 Ru S2 C3 -128.37(14) . . . . ? S1 Ru S2 C3 54.69(13) . . . . ? S3 Ru S2 C3 144.91(13) . . . . ? Cl1 Ru S2 C3 -41.01(13) . . . . ? O5 Ru S2 C4 -7.9(4) . . . . ? O4 Ru S2 C4 -19.03(15) . . . . ? S1 Ru S2 C4 164.03(14) . . . . ? S3 Ru S2 C4 -105.75(14) . . . . ? Cl1 Ru S2 C4 68.33(14) . . . . ? O5 Ru S3 O3 124.16(11) . . . . ? O4 Ru S3 O3 -153.72(11) . . . . ? S2 Ru S3 O3 -63.75(10) . . . . ? S1 Ru S3 O3 33.38(10) . . . . ? Cl1 Ru S3 O3 -178.2(2) . . . . ? O5 Ru S3 C6 -0.07(14) . . . . ? O4 Ru S3 C6 82.06(14) . . . . ? S2 Ru S3 C6 172.03(13) . . . . ? S1 Ru S3 C6 -90.84(13) . . . . ? Cl1 Ru S3 C6 57.6(3) . . . . ? O5 Ru S3 C5 -110.25(14) . . . . ? O4 Ru S3 C5 -28.13(14) . . . . ? S2 Ru S3 C5 61.84(13) . . . . ? S1 Ru S3 C5 158.97(13) . . . . ? Cl1 Ru S3 C5 -52.6(3) . . . . ? C8 S4 O4 Ru 116.44(14) . . . . ? C7 S4 O4 Ru -140.25(16) . . . . ? O5 Ru O4 S4 -42.90(12) . . . . ? S2 Ru O4 S4 135.55(12) . . . . ? S1 Ru O4 S4 -67.1(5) . . . . ? S3 Ru O4 S4 -131.39(12) . . . . ? Cl1 Ru O4 S4 45.91(12) . . . . ? C9 S5 O5 Ru -129.83(16) . . . . ? C10 S5 O5 Ru 129.28(18) . . . . ? O4 Ru O5 S5 127.13(14) . . . . ? S2 Ru O5 S5 115.9(4) . . . . ? S1 Ru O5 S5 -56.10(12) . . . . ? S3 Ru O5 S5 -145.91(12) . . . . ? Cl1 Ru O5 S5 39.59(12) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 29.64 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.438 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.069 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 828779' #TrackingRef '- Alessio- Bratsos CIF files.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H20 Cl2 N2 O2 Ru S2' _chemical_formula_weight 388.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 2/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 12.000(4) _cell_length_b 9.201(3) _cell_length_c 25.854(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.04(2) _cell_angle_gamma 90.00 _cell_volume 2854.1(14) _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 needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 1.751 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5647 _exptl_absorpt_correction_T_max 0.6946 _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_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 30772 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.10 _reflns_number_total 6083 _reflns_number_gt 4294 _reflns_threshold_expression >2\s(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 1.70.01 (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^)+(0.0303P)^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 6083 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 0.898 _refine_ls_restrained_S_all 0.898 _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 0.58552(2) 0.88856(3) 0.383042(11) 0.03814(9) Uani 1 1 d . . . Cl1 Cl 0.41909(8) 0.87218(13) 0.43415(4) 0.0607(3) Uani 1 1 d . . . Cl2 Cl 0.74960(8) 0.93482(14) 0.33477(4) 0.0645(3) Uani 1 1 d . . . S1 S 0.51480(7) 0.73774(11) 0.32240(4) 0.0445(2) Uani 1 1 d . . . S2 S 0.67175(9) 0.71413(12) 0.42787(4) 0.0599(3) Uani 1 1 d . . . O1 O 0.5147(2) 0.5795(3) 0.33274(11) 0.0630(8) Uani 1 1 d . . . O2 O 0.7412(3) 0.7660(4) 0.47219(13) 0.0917(11) Uani 1 1 d . . . N1 N 0.6464(2) 1.0460(3) 0.43725(11) 0.0467(8) Uani 1 1 d . . . H1D H 0.6343 1.0150 0.4697 0.056 Uiso 1 1 calc R . . H1E H 0.7203 1.0578 0.4335 0.056 Uiso 1 1 calc R . . N2 N 0.5169(2) 1.0803(3) 0.34880(11) 0.0461(8) Uani 1 1 d . . . H2D H 0.5266 1.0786 0.3144 0.055 Uiso 1 1 calc R . . H2E H 0.4433 1.0848 0.3547 0.055 Uiso 1 1 calc R . . C1 C 0.3750(3) 0.7840(6) 0.30451(19) 0.0815(16) Uani 1 1 d . . . H1A H 0.3479 0.7175 0.2786 0.122 Uiso 1 1 calc R . . H1B H 0.3730 0.8811 0.2910 0.122 Uiso 1 1 calc R . . H1C H 0.3287 0.7782 0.3343 0.122 Uiso 1 1 calc R . . C2 C 0.5769(4) 0.7584(5) 0.26094(15) 0.0705(13) Uani 1 1 d . . . H2A H 0.6510 0.7193 0.2622 0.106 Uiso 1 1 calc R . . H2B H 0.5799 0.8597 0.2522 0.106 Uiso 1 1 calc R . . H2C H 0.5332 0.7075 0.2353 0.106 Uiso 1 1 calc R . . C3 C 0.5818(4) 0.5808(5) 0.45411(19) 0.0812(15) Uani 1 1 d . . . H3A H 0.6248 0.5123 0.4741 0.122 Uiso 1 1 calc R . . H3B H 0.5433 0.5309 0.4265 0.122 Uiso 1 1 calc R . . H3C H 0.5285 0.6272 0.4759 0.122 Uiso 1 1 calc R . . C4 C 0.7597(4) 0.5990(5) 0.3907(2) 0.0841(16) Uani 1 1 d . . . H4A H 0.8186 0.6558 0.3763 0.126 Uiso 1 1 calc R . . H4B H 0.7167 0.5547 0.3633 0.126 Uiso 1 1 calc R . . H4C H 0.7910 0.5248 0.4126 0.126 Uiso 1 1 calc R . . C5 C 0.5886(4) 1.1858(5) 0.42832(16) 0.0582(11) Uani 1 1 d . . . H5A H 0.6323 1.2646 0.4432 0.070 Uiso 1 1 calc R . . H5B H 0.5166 1.1846 0.4448 0.070 Uiso 1 1 calc R . . C6 C 0.5735(4) 1.2085(5) 0.37158(16) 0.0619(12) Uani 1 1 d . . . H6A H 0.5292 1.2950 0.3652 0.074 Uiso 1 1 calc R . . H6B H 0.6455 1.2219 0.3558 0.074 Uiso 1 1 calc R . . Ru2 Ru 0.42740(2) 0.19756(4) 0.126421(11) 0.04111(9) Uani 1 1 d . A . Cl3 Cl 0.59789(8) 0.24313(12) 0.08015(4) 0.0575(3) Uani 1 1 d . . . Cl4 Cl 0.25946(8) 0.12466(13) 0.16730(4) 0.0606(3) Uani 1 1 d . . . S3 S 0.49816(7) 0.24925(12) 0.20495(4) 0.0475(2) Uani 1 1 d . . . S4 S 0.36765(9) 0.42469(12) 0.11024(4) 0.0550(3) Uani 1 1 d . . . O3 O 0.5277(2) 0.1178(3) 0.23588(10) 0.0681(9) Uani 1 1 d . . . O4 O 0.4097(3) 0.5466(4) 0.14284(13) 0.0917(11) Uani 1 1 d . . . C7 C 0.6186(3) 0.3621(6) 0.20541(18) 0.0836(17) Uani 1 1 d . . . H7A H 0.6405 0.3834 0.2405 0.125 Uiso 1 1 calc R . . H7B H 0.6021 0.4510 0.1874 0.125 Uiso 1 1 calc R . . H7C H 0.6783 0.3126 0.1885 0.125 Uiso 1 1 calc R . . C8 C 0.4111(3) 0.3550(5) 0.24512(15) 0.0573(11) Uani 1 1 d . . . H8A H 0.3471 0.2988 0.2545 0.086 Uiso 1 1 calc R . . H8B H 0.3871 0.4405 0.2267 0.086 Uiso 1 1 calc R . . H8C H 0.4518 0.3829 0.2758 0.086 Uiso 1 1 calc R . . C9 C 0.3946(4) 0.4783(5) 0.04570(16) 0.0679(12) Uani 1 1 d . . . H9A H 0.3600 0.5706 0.0389 0.102 Uiso 1 1 calc R . . H9B H 0.3648 0.4069 0.0222 0.102 Uiso 1 1 calc R . . H9C H 0.4736 0.4865 0.0412 0.102 Uiso 1 1 calc R . . C10 C 0.2201(4) 0.4421(6) 0.1074(2) 0.098(2) Uani 1 1 d . . . H10A H 0.1906 0.4273 0.1412 0.147 Uiso 1 1 calc R . . H10B H 0.1896 0.3707 0.0840 0.147 Uiso 1 1 calc R . . H10C H 0.2006 0.5376 0.0953 0.147 Uiso 1 1 calc R . . N3 N 0.3628(3) 0.1017(4) 0.05642(13) 0.0647(10) Uani 1 1 d . A . H3D H 0.2888 0.1175 0.0540 0.078 Uiso 1 1 calc R . . H3E H 0.3948 0.1439 0.0290 0.078 Uiso 1 1 calc R . . C11 C 0.3840(4) -0.0516(6) 0.05556(18) 0.0755(14) Uani 1 1 d . . . H11A H 0.3965 -0.0802 0.0200 0.091 Uiso 0.674(14) 1 calc PR A 1 H11B H 0.3174 -0.1013 0.0668 0.091 Uiso 0.674(14) 1 calc PR A 1 H11C H 0.3171 -0.0996 0.0427 0.091 Uiso 0.326(14) 1 calc PR A 2 H11D H 0.4421 -0.0695 0.0307 0.091 Uiso 0.326(14) 1 calc PR A 2 C12 C 0.4776(7) -0.1026(8) 0.0871(3) 0.063(2) Uiso 0.674(14) 1 d P A 1 H12A H 0.5464 -0.0891 0.0686 0.075 Uiso 0.674(14) 1 calc PR A 1 H12B H 0.4691 -0.2055 0.0942 0.075 Uiso 0.674(14) 1 calc PR A 1 C12B C 0.4161(13) -0.1187(15) 0.1025(5) 0.052(5) Uiso 0.326(14) 1 d P A 2 H12C H 0.4601 -0.2045 0.0952 0.063 Uiso 0.326(14) 1 calc PR A 2 H12D H 0.3500 -0.1496 0.1205 0.063 Uiso 0.326(14) 1 calc PR A 2 N4 N 0.4823(2) -0.0197(3) 0.13664(12) 0.0502(8) Uani 1 1 d . . . H4D H 0.5528 -0.0195 0.1491 0.060 Uiso 0.674(14) 1 calc PR A 1 H4E H 0.4392 -0.0641 0.1600 0.060 Uiso 0.674(14) 1 calc PR A 1 H4F H 0.5550 -0.0263 0.1289 0.060 Uiso 0.326(14) 1 calc PR A 2 H4G H 0.4744 -0.0462 0.1699 0.060 Uiso 0.326(14) 1 calc PR 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 Ru1 0.04134(15) 0.03788(19) 0.03514(16) -0.00261(12) -0.00069(11) 0.00074(12) Cl1 0.0577(5) 0.0776(9) 0.0472(6) -0.0017(5) 0.0140(4) -0.0082(5) Cl2 0.0447(5) 0.0853(9) 0.0638(7) -0.0166(6) 0.0115(4) -0.0102(5) S1 0.0485(5) 0.0450(6) 0.0399(5) -0.0058(4) -0.0037(4) -0.0015(4) S2 0.0794(7) 0.0415(7) 0.0579(7) -0.0058(5) -0.0258(5) 0.0098(5) O1 0.088(2) 0.0378(19) 0.0628(19) -0.0035(14) -0.0168(15) -0.0099(14) O2 0.131(3) 0.054(2) 0.087(2) -0.0117(18) -0.069(2) 0.0149(19) N1 0.0576(17) 0.044(2) 0.0389(18) -0.0040(14) -0.0026(13) -0.0007(15) N2 0.0509(17) 0.046(2) 0.0415(18) 0.0014(14) -0.0012(13) 0.0060(14) C1 0.061(3) 0.099(4) 0.084(4) -0.036(3) -0.028(2) 0.014(3) C2 0.093(3) 0.078(4) 0.041(2) -0.015(2) 0.009(2) -0.018(3) C3 0.136(4) 0.038(3) 0.069(3) 0.015(2) -0.001(3) 0.002(3) C4 0.080(3) 0.064(4) 0.108(4) -0.020(3) -0.019(3) 0.030(3) C5 0.081(3) 0.042(3) 0.052(3) -0.007(2) -0.004(2) 0.011(2) C6 0.085(3) 0.046(3) 0.054(3) 0.001(2) -0.007(2) 0.005(2) Ru2 0.04378(16) 0.0439(2) 0.03559(17) -0.00139(13) -0.00086(11) -0.00234(13) Cl3 0.0569(5) 0.0628(7) 0.0533(6) 0.0013(5) 0.0150(4) -0.0018(5) Cl4 0.0455(5) 0.0681(8) 0.0684(7) -0.0044(6) 0.0059(4) -0.0128(5) S3 0.0466(5) 0.0585(7) 0.0372(5) -0.0036(4) -0.0012(4) -0.0050(4) S4 0.0688(6) 0.0484(7) 0.0477(6) 0.0013(5) 0.0007(5) 0.0047(5) O3 0.090(2) 0.071(2) 0.0430(17) 0.0043(15) -0.0085(14) 0.0199(17) O4 0.164(3) 0.047(2) 0.063(2) -0.0105(17) -0.024(2) -0.002(2) C7 0.060(3) 0.125(5) 0.066(3) -0.026(3) 0.000(2) -0.041(3) C8 0.067(2) 0.065(3) 0.039(2) -0.015(2) 0.0020(18) -0.005(2) C9 0.093(3) 0.061(3) 0.050(3) 0.014(2) -0.006(2) 0.001(3) C10 0.073(3) 0.099(5) 0.123(5) 0.032(4) 0.021(3) 0.036(3) N3 0.080(2) 0.065(3) 0.048(2) -0.0109(18) -0.0166(17) 0.0108(19) C11 0.090(3) 0.070(4) 0.065(3) -0.019(3) -0.015(2) 0.016(3) N4 0.0556(17) 0.051(2) 0.0442(19) 0.0003(16) -0.0047(14) -0.0012(16) _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 Ru1 N2 2.132(3) . ? Ru1 N1 2.135(3) . ? Ru1 S2 2.2240(12) . ? Ru1 S1 2.2485(11) . ? Ru1 Cl2 2.3885(12) . ? Ru1 Cl1 2.4193(11) . ? S1 O1 1.480(3) . ? S1 C2 1.777(4) . ? S1 C1 1.784(4) . ? S2 O2 1.483(3) . ? S2 C3 1.777(5) . ? S2 C4 1.787(4) . ? N1 C5 1.478(5) . ? N2 C6 1.479(5) . ? C5 C6 1.489(5) . ? Ru2 N4 2.120(3) . ? Ru2 N3 2.146(3) . ? Ru2 S3 2.2375(11) . ? Ru2 S4 2.2462(13) . ? Ru2 Cl4 2.3886(12) . ? Ru2 Cl3 2.4252(11) . ? S3 O3 1.489(3) . ? S3 C8 1.777(4) . ? S3 C7 1.780(4) . ? S4 O4 1.486(3) . ? S4 C9 1.775(4) . ? S4 C10 1.778(4) . ? N3 C11 1.433(5) . ? C11 C12B 1.410(13) . ? C11 C12 1.453(8) . ? C12 N4 1.492(7) . ? C12B N4 1.487(13) . ? 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 Ru1 N1 80.58(12) . . ? N2 Ru1 S2 170.34(9) . . ? N1 Ru1 S2 89.83(9) . . ? N2 Ru1 S1 94.77(9) . . ? N1 Ru1 S1 175.34(9) . . ? S2 Ru1 S1 94.83(5) . . ? N2 Ru1 Cl2 87.22(8) . . ? N1 Ru1 Cl2 86.94(8) . . ? S2 Ru1 Cl2 91.18(5) . . ? S1 Ru1 Cl2 92.86(4) . . ? N2 Ru1 Cl1 87.81(8) . . ? N1 Ru1 Cl1 87.69(8) . . ? S2 Ru1 Cl1 92.94(5) . . ? S1 Ru1 Cl1 92.16(4) . . ? Cl2 Ru1 Cl1 173.22(4) . . ? O1 S1 C2 105.6(2) . . ? O1 S1 C1 106.1(2) . . ? C2 S1 C1 98.6(2) . . ? O1 S1 Ru1 118.86(12) . . ? C2 S1 Ru1 113.47(15) . . ? C1 S1 Ru1 112.02(15) . . ? O2 S2 C3 105.3(2) . . ? O2 S2 C4 106.1(2) . . ? C3 S2 C4 99.5(2) . . ? O2 S2 Ru1 114.82(14) . . ? C3 S2 Ru1 114.64(17) . . ? C4 S2 Ru1 114.92(18) . . ? C5 N1 Ru1 109.5(2) . . ? C6 N2 Ru1 108.9(2) . . ? N1 C5 C6 108.9(3) . . ? N2 C6 C5 109.1(3) . . ? N4 Ru2 N3 79.88(13) . . ? N4 Ru2 S3 88.59(9) . . ? N3 Ru2 S3 167.99(11) . . ? N4 Ru2 S4 176.37(9) . . ? N3 Ru2 S4 96.66(10) . . ? S3 Ru2 S4 94.92(4) . . ? N4 Ru2 Cl4 86.72(9) . . ? N3 Ru2 Cl4 87.87(11) . . ? S3 Ru2 Cl4 88.14(4) . . ? S4 Ru2 Cl4 94.28(4) . . ? N4 Ru2 Cl3 87.79(9) . . ? N3 Ru2 Cl3 87.15(11) . . ? S3 Ru2 Cl3 95.81(4) . . ? S4 Ru2 Cl3 90.95(4) . . ? Cl4 Ru2 Cl3 173.16(4) . . ? O3 S3 C8 105.52(19) . . ? O3 S3 C7 106.5(2) . . ? C8 S3 C7 99.4(2) . . ? O3 S3 Ru2 113.42(13) . . ? C8 S3 Ru2 115.41(14) . . ? C7 S3 Ru2 115.14(16) . . ? O4 S4 C9 104.9(2) . . ? O4 S4 C10 106.4(3) . . ? C9 S4 C10 97.7(2) . . ? O4 S4 Ru2 119.53(15) . . ? C9 S4 Ru2 111.75(16) . . ? C10 S4 Ru2 113.94(19) . . ? C11 N3 Ru2 110.8(3) . . ? C12B C11 N3 117.6(7) . . ? C12B C11 C12 34.8(5) . . ? N3 C11 C12 116.4(5) . . ? C11 C12 N4 109.5(5) . . ? C11 C12B N4 112.2(10) . . ? C12B N4 C12 33.5(5) . . ? C12B N4 Ru2 110.0(5) . . ? C12 N4 Ru2 111.6(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 N2 Ru1 S1 O1 -166.03(16) . . . . ? N1 Ru1 S1 O1 -166.1(10) . . . . ? S2 Ru1 S1 O1 15.10(15) . . . . ? Cl2 Ru1 S1 O1 106.53(15) . . . . ? Cl1 Ru1 S1 O1 -78.04(15) . . . . ? N2 Ru1 S1 C2 69.0(2) . . . . ? N1 Ru1 S1 C2 68.9(10) . . . . ? S2 Ru1 S1 C2 -109.90(19) . . . . ? Cl2 Ru1 S1 C2 -18.47(19) . . . . ? Cl1 Ru1 S1 C2 156.96(19) . . . . ? N2 Ru1 S1 C1 -41.6(2) . . . . ? N1 Ru1 S1 C1 -41.7(10) . . . . ? S2 Ru1 S1 C1 139.5(2) . . . . ? Cl2 Ru1 S1 C1 -129.1(2) . . . . ? Cl1 Ru1 S1 C1 46.3(2) . . . . ? N2 Ru1 S2 O2 2.1(6) . . . . ? N1 Ru1 S2 O2 -4.5(2) . . . . ? S1 Ru1 S2 O2 175.43(19) . . . . ? Cl2 Ru1 S2 O2 82.46(19) . . . . ? Cl1 Ru1 S2 O2 -92.15(19) . . . . ? N2 Ru1 S2 C3 124.3(5) . . . . ? N1 Ru1 S2 C3 117.7(2) . . . . ? S1 Ru1 S2 C3 -62.44(19) . . . . ? Cl2 Ru1 S2 C3 -155.41(19) . . . . ? Cl1 Ru1 S2 C3 29.98(19) . . . . ? N2 Ru1 S2 C4 -121.3(5) . . . . ? N1 Ru1 S2 C4 -127.9(2) . . . . ? S1 Ru1 S2 C4 51.97(19) . . . . ? Cl2 Ru1 S2 C4 -41.00(19) . . . . ? Cl1 Ru1 S2 C4 144.38(19) . . . . ? N2 Ru1 N1 C5 12.7(2) . . . . ? S2 Ru1 N1 C5 -168.4(2) . . . . ? S1 Ru1 N1 C5 12.8(12) . . . . ? Cl2 Ru1 N1 C5 100.4(2) . . . . ? Cl1 Ru1 N1 C5 -75.4(2) . . . . ? N1 Ru1 N2 C6 15.6(2) . . . . ? S2 Ru1 N2 C6 8.9(7) . . . . ? S1 Ru1 N2 C6 -164.4(2) . . . . ? Cl2 Ru1 N2 C6 -71.8(2) . . . . ? Cl1 Ru1 N2 C6 103.6(2) . . . . ? Ru1 N1 C5 C6 -38.9(4) . . . . ? Ru1 N2 C6 C5 -41.5(4) . . . . ? N1 C5 C6 N2 53.9(4) . . . . ? N4 Ru2 S3 O3 -13.13(15) . . . . ? N3 Ru2 S3 O3 3.0(5) . . . . ? S4 Ru2 S3 O3 167.78(13) . . . . ? Cl4 Ru2 S3 O3 73.64(13) . . . . ? Cl3 Ru2 S3 O3 -100.76(13) . . . . ? N4 Ru2 S3 C8 -135.04(18) . . . . ? N3 Ru2 S3 C8 -118.9(5) . . . . ? S4 Ru2 S3 C8 45.86(17) . . . . ? Cl4 Ru2 S3 C8 -48.27(17) . . . . ? Cl3 Ru2 S3 C8 137.32(17) . . . . ? N4 Ru2 S3 C7 110.0(2) . . . . ? N3 Ru2 S3 C7 126.1(5) . . . . ? S4 Ru2 S3 C7 -69.1(2) . . . . ? Cl4 Ru2 S3 C7 -163.3(2) . . . . ? Cl3 Ru2 S3 C7 22.3(2) . . . . ? N4 Ru2 S4 O4 -150.4(14) . . . . ? N3 Ru2 S4 O4 -168.0(2) . . . . ? S3 Ru2 S4 O4 15.13(18) . . . . ? Cl4 Ru2 S4 O4 103.63(18) . . . . ? Cl3 Ru2 S4 O4 -80.78(18) . . . . ? N4 Ru2 S4 C9 -27.4(14) . . . . ? N3 Ru2 S4 C9 -45.0(2) . . . . ? S3 Ru2 S4 C9 138.15(17) . . . . ? Cl4 Ru2 S4 C9 -133.35(17) . . . . ? Cl3 Ru2 S4 C9 42.24(17) . . . . ? N4 Ru2 S4 C10 82.2(14) . . . . ? N3 Ru2 S4 C10 64.6(2) . . . . ? S3 Ru2 S4 C10 -112.3(2) . . . . ? Cl4 Ru2 S4 C10 -23.8(2) . . . . ? Cl3 Ru2 S4 C10 151.8(2) . . . . ? N4 Ru2 N3 C11 3.5(3) . . . . ? S3 Ru2 N3 C11 -12.9(7) . . . . ? S4 Ru2 N3 C11 -177.6(3) . . . . ? Cl4 Ru2 N3 C11 -83.6(3) . . . . ? Cl3 Ru2 N3 C11 91.7(3) . . . . ? Ru2 N3 C11 C12B 14.8(9) . . . . ? Ru2 N3 C11 C12 -24.4(6) . . . . ? C12B C11 C12 N4 -62.5(11) . . . . ? N3 C11 C12 N4 38.5(8) . . . . ? N3 C11 C12B N4 -32.4(14) . . . . ? C12 C11 C12B N4 65.0(11) . . . . ? C11 C12B N4 C12 -66.1(11) . . . . ? C11 C12B N4 Ru2 33.1(12) . . . . ? C11 C12 N4 C12B 60.6(10) . . . . ? C11 C12 N4 Ru2 -33.3(7) . . . . ? N3 Ru2 N4 C12B -19.4(7) . . . . ? S3 Ru2 N4 C12B 157.2(7) . . . . ? S4 Ru2 N4 C12B -37.2(16) . . . . ? Cl4 Ru2 N4 C12B 69.0(7) . . . . ? Cl3 Ru2 N4 C12B -106.9(7) . . . . ? N3 Ru2 N4 C12 16.5(4) . . . . ? S3 Ru2 N4 C12 -166.9(4) . . . . ? S4 Ru2 N4 C12 -1.3(16) . . . . ? Cl4 Ru2 N4 C12 104.9(4) . . . . ? Cl3 Ru2 N4 C12 -71.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.437 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.094 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 828780' #TrackingRef '- Alessio- Bratsos CIF files.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H44 Cl4 N2 O6 Ru2 S6' _chemical_formula_weight 872.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0074 0.0035 '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 0.0136 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0227 0.0128 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.2073 0.2439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.2413 0.3112 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -0.5010 1.5477 '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 bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.3210(11) _cell_length_b 26.898(3) _cell_length_c 16.1320(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6214.1(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.21 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_max 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3536 _exptl_absorpt_coefficient_mu 4.315 _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 100(2) _diffrn_radiation_wavelength 1.00000 _diffrn_radiation_type synchrotron _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 22588 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.44 _reflns_number_total 2294 _reflns_number_gt 2063 _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 'SHELX97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX97 (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^)+(0.0401P)^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 2294 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0688 _refine_ls_wR_factor_gt 0.0663 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _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 0.04175(3) 0.276218(15) 0.32672(2) 0.0164(2) Uani 1 1 d . . . Ru2 Ru -0.26814(3) 0.479266(15) 0.33356(2) 0.0162(2) Uani 1 1 d . . . Cl1 Cl 0.15506(9) 0.30294(5) 0.22441(7) 0.0242(4) Uani 1 1 d . . . Cl2 Cl -0.05014(8) 0.24174(5) 0.21419(7) 0.0225(4) Uani 1 1 d . . . Cl3 Cl -0.17989(9) 0.51690(5) 0.22121(7) 0.0254(4) Uani 1 1 d . . . Cl4 Cl -0.38377(9) 0.45480(5) 0.23059(7) 0.0219(4) Uani 1 1 d . . . S1 S 0.12662(9) 0.30727(5) 0.43255(8) 0.0227(4) Uani 1 1 d . . . S2 S -0.07708(9) 0.25997(5) 0.41594(8) 0.0225(4) Uani 1 1 d . . . S3 S 0.10907(9) 0.19915(5) 0.33210(8) 0.0218(4) Uani 1 1 d . . . S4 S -0.14835(9) 0.49319(5) 0.42204(8) 0.0210(4) Uani 1 1 d . . . S5 S -0.35136(9) 0.44452(5) 0.43803(8) 0.0228(4) Uani 1 1 d . . . S6 S -0.33627(10) 0.55591(5) 0.34777(8) 0.0237(4) Uani 1 1 d . . . O1 O 0.1573(2) 0.27204(12) 0.4966(2) 0.0353(11) Uani 1 1 d . . . O2 O -0.1258(2) 0.30616(12) 0.4421(2) 0.0296(10) Uani 1 1 d . . . O3 O 0.0611(2) 0.16076(12) 0.3826(2) 0.0264(10) Uani 1 1 d . . . O4 O -0.0935(2) 0.44720(12) 0.44162(19) 0.0252(9) Uani 1 1 d . . . O5 O -0.3749(3) 0.47698(14) 0.5081(2) 0.0411(11) Uani 1 1 d . . . O6 O -0.2852(2) 0.59367(12) 0.3968(2) 0.0336(10) Uani 1 1 d . . . N1 N -0.0212(3) 0.34728(14) 0.3093(2) 0.0165(11) Uani 1 1 d . . . H1A H -0.0490 0.3562 0.3585 0.020 Uiso 1 1 calc R . . H1B H 0.0258 0.3698 0.2995 0.020 Uiso 1 1 calc R . . N2 N -0.2053(3) 0.40909(14) 0.3098(2) 0.0153(11) Uani 1 1 d . . . H2A H -0.1779 0.3986 0.3583 0.018 Uiso 1 1 calc R . . H2B H -0.2525 0.3870 0.2980 0.018 Uiso 1 1 calc R . . C1 C 0.2267(3) 0.34128(19) 0.4022(3) 0.0305(15) Uani 1 1 d . . . H1C H 0.2687 0.3196 0.3707 0.046 Uiso 1 1 calc R . . H1D H 0.2591 0.3536 0.4516 0.046 Uiso 1 1 calc R . . H1E H 0.2078 0.3695 0.3676 0.046 Uiso 1 1 calc R . . C2 C 0.0687(4) 0.3557(2) 0.4883(3) 0.0359(16) Uani 1 1 d . . . H2C H 0.1085 0.3668 0.5341 0.054 Uiso 1 1 calc R . . H2D H 0.0096 0.3431 0.5105 0.054 Uiso 1 1 calc R . . H2E H 0.0564 0.3836 0.4510 0.054 Uiso 1 1 calc R . . C3 C -0.1647(3) 0.21963(18) 0.3782(3) 0.0255(15) Uani 1 1 d . . . H3A H -0.1910 0.2333 0.3269 0.038 Uiso 1 1 calc R . . H3B H -0.2143 0.2164 0.4198 0.038 Uiso 1 1 calc R . . H3C H -0.1375 0.1869 0.3670 0.038 Uiso 1 1 calc R . . C4 C -0.0477(4) 0.22727(18) 0.5077(3) 0.0307(16) Uani 1 1 d . . . H4A H -0.1029 0.2247 0.5433 0.046 Uiso 1 1 calc R . . H4B H 0.0018 0.2452 0.5371 0.046 Uiso 1 1 calc R . . H4C H -0.0257 0.1939 0.4932 0.046 Uiso 1 1 calc R . . C5 C 0.1239(4) 0.17251(18) 0.2317(3) 0.0259(15) Uani 1 1 d . . . H5A H 0.0626 0.1652 0.2076 0.039 Uiso 1 1 calc R . . H5B H 0.1599 0.1417 0.2363 0.039 Uiso 1 1 calc R . . H5C H 0.1573 0.1960 0.1960 0.039 Uiso 1 1 calc R . . C6 C 0.2278(3) 0.2002(2) 0.3630(3) 0.0268(15) Uani 1 1 d . . . H6A H 0.2553 0.1672 0.3549 0.040 Uiso 1 1 calc R . . H6B H 0.2319 0.2094 0.4217 0.040 Uiso 1 1 calc R . . H6C H 0.2618 0.2247 0.3295 0.040 Uiso 1 1 calc R . . C7 C -0.0656(3) 0.53716(19) 0.3858(3) 0.0262(15) Uani 1 1 d . . . H7A H -0.0339 0.5239 0.3367 0.039 Uiso 1 1 calc R . . H7B H -0.0196 0.5437 0.4293 0.039 Uiso 1 1 calc R . . H7C H -0.0977 0.5682 0.3713 0.039 Uiso 1 1 calc R . . C8 C -0.1774(4) 0.52035(18) 0.5191(3) 0.0247(14) Uani 1 1 d . . . H8A H -0.1201 0.5274 0.5501 0.037 Uiso 1 1 calc R . . H8B H -0.2164 0.4972 0.5509 0.037 Uiso 1 1 calc R . . H8C H -0.2117 0.5514 0.5099 0.037 Uiso 1 1 calc R . . C9 C -0.2963(4) 0.39089(19) 0.4810(3) 0.0385(17) Uani 1 1 d . . . H9A H -0.3328 0.3789 0.5283 0.058 Uiso 1 1 calc R . . H9B H -0.2332 0.3996 0.4995 0.058 Uiso 1 1 calc R . . H9C H -0.2927 0.3648 0.4388 0.058 Uiso 1 1 calc R . . C10 C -0.4567(4) 0.4152(2) 0.4063(3) 0.0355(16) Uani 1 1 d . . . H10A H -0.5001 0.4404 0.3852 0.053 Uiso 1 1 calc R . . H10B H -0.4849 0.3981 0.4538 0.053 Uiso 1 1 calc R . . H10C H -0.4431 0.3910 0.3625 0.053 Uiso 1 1 calc R . . C11 C -0.4524(4) 0.5536(2) 0.3839(3) 0.0394(17) Uani 1 1 d . . . H11A H -0.4804 0.5867 0.3800 0.059 Uiso 1 1 calc R . . H11B H -0.4529 0.5426 0.4418 0.059 Uiso 1 1 calc R . . H11C H -0.4883 0.5302 0.3500 0.059 Uiso 1 1 calc R . . C12 C -0.3603(4) 0.58348(18) 0.2494(3) 0.0325(15) Uani 1 1 d . . . H12A H -0.3014 0.5906 0.2208 0.049 Uiso 1 1 calc R . . H12B H -0.3951 0.6145 0.2575 0.049 Uiso 1 1 calc R . . H12C H -0.3977 0.5605 0.2159 0.049 Uiso 1 1 calc R . . C13 C -0.0917(3) 0.35322(18) 0.2426(3) 0.0199(14) Uani 1 1 d . . . H13A H -0.1416 0.3281 0.2500 0.024 Uiso 1 1 calc R . . H13B H -0.0618 0.3472 0.1882 0.024 Uiso 1 1 calc R . . C14 C -0.1345(3) 0.40459(18) 0.2432(3) 0.0205(14) Uani 1 1 d . . . H14A H -0.0849 0.4297 0.2518 0.025 Uiso 1 1 calc R . . H14B H -0.1642 0.4112 0.1889 0.025 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 0.0147(3) 0.0153(4) 0.0193(3) -0.00026(19) -0.0009(2) -0.0005(2) Ru2 0.0148(3) 0.0149(4) 0.0190(3) 0.00023(19) 0.00027(19) 0.0003(2) Cl1 0.0229(9) 0.0225(9) 0.0271(9) 0.0012(6) 0.0049(7) -0.0020(7) Cl2 0.0218(8) 0.0235(9) 0.0222(8) -0.0019(7) -0.0029(6) -0.0004(7) Cl3 0.0245(9) 0.0249(9) 0.0267(9) 0.0045(7) 0.0024(7) -0.0023(7) Cl4 0.0203(9) 0.0218(9) 0.0237(8) 0.0006(7) -0.0026(6) -0.0011(7) S1 0.0214(9) 0.0205(10) 0.0262(9) -0.0020(8) -0.0041(7) -0.0015(8) S2 0.0220(9) 0.0219(10) 0.0235(9) -0.0035(7) 0.0017(7) -0.0013(8) S3 0.0182(9) 0.0172(10) 0.0300(9) 0.0008(7) -0.0007(7) -0.0006(8) S4 0.0206(9) 0.0202(10) 0.0221(9) -0.0013(7) 0.0000(7) -0.0019(8) S5 0.0211(9) 0.0234(10) 0.0240(9) -0.0002(8) 0.0035(7) -0.0028(8) S6 0.0234(10) 0.0165(10) 0.0311(9) -0.0007(7) -0.0011(7) 0.0016(8) O1 0.036(3) 0.036(3) 0.034(2) 0.007(2) -0.0117(19) -0.002(2) O2 0.032(2) 0.018(2) 0.038(2) -0.0055(19) 0.0139(18) 0.004(2) O3 0.022(2) 0.017(2) 0.039(2) 0.0103(19) 0.0014(18) -0.0037(19) O4 0.025(2) 0.022(2) 0.029(2) -0.0008(18) -0.0095(17) 0.008(2) O5 0.044(3) 0.042(3) 0.038(3) -0.007(2) 0.008(2) -0.003(2) O6 0.044(3) 0.014(2) 0.043(2) -0.0092(19) -0.013(2) 0.000(2) N1 0.014(3) 0.012(3) 0.023(3) 0.000(2) 0.001(2) -0.001(2) N2 0.014(3) 0.008(3) 0.023(3) -0.002(2) -0.001(2) 0.003(2) C1 0.026(4) 0.034(4) 0.031(4) 0.003(3) -0.003(3) -0.006(3) C2 0.038(4) 0.036(4) 0.034(4) -0.013(3) -0.001(3) 0.000(3) C3 0.017(4) 0.032(4) 0.027(3) 0.001(3) 0.007(3) -0.003(3) C4 0.037(4) 0.035(4) 0.021(3) 0.004(3) 0.002(3) -0.013(3) C5 0.027(4) 0.016(3) 0.035(4) -0.012(3) 0.002(3) 0.008(3) C6 0.019(4) 0.024(4) 0.038(4) 0.000(3) -0.001(3) 0.001(3) C7 0.022(4) 0.029(4) 0.028(3) -0.006(3) -0.003(3) -0.009(3) C8 0.029(4) 0.020(4) 0.025(3) -0.006(3) -0.003(3) -0.002(3) C9 0.044(4) 0.032(4) 0.040(4) 0.023(3) 0.013(3) 0.007(3) C10 0.040(4) 0.036(4) 0.031(4) 0.000(3) 0.006(3) -0.020(3) C11 0.037(4) 0.026(4) 0.055(4) 0.003(3) 0.011(3) 0.014(3) C12 0.042(4) 0.019(4) 0.037(4) 0.005(3) -0.012(3) 0.001(3) C13 0.015(3) 0.021(4) 0.024(3) 0.004(3) -0.001(3) -0.001(3) C14 0.017(3) 0.020(4) 0.024(3) -0.003(3) 0.001(3) 0.001(3) _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 Ru1 N1 2.132(4) . ? Ru1 S1 2.2561(13) . ? Ru1 S2 2.2712(13) . ? Ru1 S3 2.2879(14) . ? Ru1 Cl1 2.4236(13) . ? Ru1 Cl2 2.4264(12) . ? Ru2 N2 2.126(4) . ? Ru2 S4 2.2630(13) . ? Ru2 S5 2.2659(13) . ? Ru2 S6 2.2923(14) . ? Ru2 Cl3 2.4304(13) . ? Ru2 Cl4 2.4361(12) . ? S1 O1 1.469(3) . ? S1 C1 1.769(5) . ? S1 C2 1.787(5) . ? S2 O2 1.486(3) . ? S2 C3 1.767(5) . ? S2 C4 1.772(5) . ? S3 O3 1.484(3) . ? S3 C6 1.772(5) . ? S3 C5 1.784(5) . ? S4 O4 1.499(3) . ? S4 C7 1.773(5) . ? S4 C8 1.778(5) . ? S5 O5 1.468(4) . ? S5 C10 1.777(5) . ? S5 C9 1.784(5) . ? S6 O6 1.481(3) . ? S6 C11 1.763(5) . ? S6 C12 1.785(5) . ? N1 C13 1.483(6) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C14 1.482(6) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C1 H1E 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C2 H2E 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.512(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 S1 89.77(11) . . ? N1 Ru1 S2 86.51(11) . . ? S1 Ru1 S2 89.73(5) . . ? N1 Ru1 S3 174.57(11) . . ? S1 Ru1 S3 94.58(5) . . ? S2 Ru1 S3 96.74(5) . . ? N1 Ru1 Cl1 85.84(11) . . ? S1 Ru1 Cl1 92.57(5) . . ? S2 Ru1 Cl1 172.00(5) . . ? S3 Ru1 Cl1 90.71(5) . . ? N1 Ru1 Cl2 90.82(10) . . ? S1 Ru1 Cl2 179.14(5) . . ? S2 Ru1 Cl2 89.67(5) . . ? S3 Ru1 Cl2 84.87(5) . . ? Cl1 Ru1 Cl2 88.11(4) . . ? N2 Ru2 S4 86.55(11) . . ? N2 Ru2 S5 89.45(11) . . ? S4 Ru2 S5 89.87(5) . . ? N2 Ru2 S6 175.35(11) . . ? S4 Ru2 S6 96.36(5) . . ? S5 Ru2 S6 94.17(5) . . ? N2 Ru2 Cl3 90.88(11) . . ? S4 Ru2 Cl3 90.41(5) . . ? S5 Ru2 Cl3 179.58(5) . . ? S6 Ru2 Cl3 85.49(5) . . ? N2 Ru2 Cl4 85.69(11) . . ? S4 Ru2 Cl4 171.95(5) . . ? S5 Ru2 Cl4 92.19(5) . . ? S6 Ru2 Cl4 91.25(5) . . ? Cl3 Ru2 Cl4 87.57(4) . . ? O1 S1 C1 106.6(2) . . ? O1 S1 C2 104.8(2) . . ? C1 S1 C2 98.0(3) . . ? O1 S1 Ru1 117.00(15) . . ? C1 S1 Ru1 114.74(18) . . ? C2 S1 Ru1 113.65(18) . . ? O2 S2 C3 106.1(2) . . ? O2 S2 C4 106.9(2) . . ? C3 S2 C4 98.7(2) . . ? O2 S2 Ru1 111.76(15) . . ? C3 S2 Ru1 115.59(17) . . ? C4 S2 Ru1 116.52(19) . . ? O3 S3 C6 107.6(2) . . ? O3 S3 C5 105.9(2) . . ? C6 S3 C5 98.5(2) . . ? O3 S3 Ru1 117.15(14) . . ? C6 S3 Ru1 113.57(19) . . ? C5 S3 Ru1 112.31(17) . . ? O4 S4 C7 105.7(2) . . ? O4 S4 C8 106.0(2) . . ? C7 S4 C8 100.0(2) . . ? O4 S4 Ru2 113.18(14) . . ? C7 S4 Ru2 114.12(17) . . ? C8 S4 Ru2 116.51(18) . . ? O5 S5 C10 106.9(2) . . ? O5 S5 C9 106.4(2) . . ? C10 S5 C9 97.4(3) . . ? O5 S5 Ru2 116.66(16) . . ? C10 S5 Ru2 114.54(18) . . ? C9 S5 Ru2 112.96(18) . . ? O6 S6 C11 108.3(2) . . ? O6 S6 C12 106.6(2) . . ? C11 S6 C12 97.3(3) . . ? O6 S6 Ru2 117.41(15) . . ? C11 S6 Ru2 113.74(19) . . ? C12 S6 Ru2 111.52(18) . . ? C13 N1 Ru1 118.7(3) . . ? C13 N1 H1A 107.6 . . ? Ru1 N1 H1A 107.6 . . ? C13 N1 H1B 107.6 . . ? Ru1 N1 H1B 107.6 . . ? H1A N1 H1B 107.1 . . ? C14 N2 Ru2 119.5(3) . . ? C14 N2 H2A 107.4 . . ? Ru2 N2 H2A 107.4 . . ? C14 N2 H2B 107.4 . . ? Ru2 N2 H2B 107.4 . . ? H2A N2 H2B 107.0 . . ? S1 C1 H1C 109.5 . . ? S1 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? S1 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? S1 C2 H2C 109.5 . . ? S1 C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? S1 C2 H2E 109.5 . . ? H2C C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? S2 C3 H3A 109.5 . . ? S2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? S2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? S2 C4 H4A 109.5 . . ? S2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? S3 C5 H5A 109.5 . . ? S3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? S3 C6 H6A 109.5 . . ? S3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? S3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? S4 C7 H7A 109.5 . . ? S4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? S4 C8 H8A 109.5 . . ? S4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? S5 C9 H9A 109.5 . . ? S5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? S5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? S5 C10 H10A 109.5 . . ? S5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? S5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? S6 C11 H11A 109.5 . . ? S6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? S6 C12 H12A 109.5 . . ? S6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 111.7(4) . . ? N1 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? N1 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? N2 C14 C13 110.9(4) . . ? N2 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? 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 N1 Ru1 S1 O1 153.8(2) . . . . ? S2 Ru1 S1 O1 67.30(18) . . . . ? S3 Ru1 S1 O1 -29.43(18) . . . . ? Cl1 Ru1 S1 O1 -120.36(18) . . . . ? Cl2 Ru1 S1 O1 21(3) . . . . ? N1 Ru1 S1 C1 -80.1(2) . . . . ? S2 Ru1 S1 C1 -166.7(2) . . . . ? S3 Ru1 S1 C1 96.6(2) . . . . ? Cl1 Ru1 S1 C1 5.7(2) . . . . ? Cl2 Ru1 S1 C1 147(3) . . . . ? N1 Ru1 S1 C2 31.5(2) . . . . ? S2 Ru1 S1 C2 -55.1(2) . . . . ? S3 Ru1 S1 C2 -151.8(2) . . . . ? Cl1 Ru1 S1 C2 117.3(2) . . . . ? Cl2 Ru1 S1 C2 -101(3) . . . . ? N1 Ru1 S2 O2 -16.64(19) . . . . ? S1 Ru1 S2 O2 73.14(16) . . . . ? S3 Ru1 S2 O2 167.72(16) . . . . ? Cl1 Ru1 S2 O2 -33.6(4) . . . . ? Cl2 Ru1 S2 O2 -107.48(16) . . . . ? N1 Ru1 S2 C3 104.8(2) . . . . ? S1 Ru1 S2 C3 -165.4(2) . . . . ? S3 Ru1 S2 C3 -70.8(2) . . . . ? Cl1 Ru1 S2 C3 87.8(4) . . . . ? Cl2 Ru1 S2 C3 14.0(2) . . . . ? N1 Ru1 S2 C4 -139.9(2) . . . . ? S1 Ru1 S2 C4 -50.1(2) . . . . ? S3 Ru1 S2 C4 44.5(2) . . . . ? Cl1 Ru1 S2 C4 -156.9(4) . . . . ? Cl2 Ru1 S2 C4 129.3(2) . . . . ? N1 Ru1 S3 O3 -123.3(11) . . . . ? S1 Ru1 S3 O3 93.60(16) . . . . ? S2 Ru1 S3 O3 3.33(17) . . . . ? Cl1 Ru1 S3 O3 -173.77(16) . . . . ? Cl2 Ru1 S3 O3 -85.73(16) . . . . ? N1 Ru1 S3 C6 110.3(12) . . . . ? S1 Ru1 S3 C6 -32.8(2) . . . . ? S2 Ru1 S3 C6 -123.1(2) . . . . ? Cl1 Ru1 S3 C6 59.8(2) . . . . ? Cl2 Ru1 S3 C6 147.8(2) . . . . ? N1 Ru1 S3 C5 -0.4(12) . . . . ? S1 Ru1 S3 C5 -143.52(19) . . . . ? S2 Ru1 S3 C5 126.21(19) . . . . ? Cl1 Ru1 S3 C5 -50.88(19) . . . . ? Cl2 Ru1 S3 C5 37.15(19) . . . . ? N2 Ru2 S4 O4 -13.35(18) . . . . ? S5 Ru2 S4 O4 76.11(16) . . . . ? S6 Ru2 S4 O4 170.29(15) . . . . ? Cl3 Ru2 S4 O4 -104.20(16) . . . . ? Cl4 Ru2 S4 O4 -28.8(4) . . . . ? N2 Ru2 S4 C7 107.6(2) . . . . ? S5 Ru2 S4 C7 -163.0(2) . . . . ? S6 Ru2 S4 C7 -68.8(2) . . . . ? Cl3 Ru2 S4 C7 16.7(2) . . . . ? Cl4 Ru2 S4 C7 92.1(4) . . . . ? N2 Ru2 S4 C8 -136.7(2) . . . . ? S5 Ru2 S4 C8 -47.2(2) . . . . ? S6 Ru2 S4 C8 47.0(2) . . . . ? Cl3 Ru2 S4 C8 132.5(2) . . . . ? Cl4 Ru2 S4 C8 -152.1(4) . . . . ? N2 Ru2 S5 O5 149.3(2) . . . . ? S4 Ru2 S5 O5 62.74(18) . . . . ? S6 Ru2 S5 O5 -33.62(18) . . . . ? Cl3 Ru2 S5 O5 -69(8) . . . . ? Cl4 Ru2 S5 O5 -125.04(18) . . . . ? N2 Ru2 S5 C10 -84.8(2) . . . . ? S4 Ru2 S5 C10 -171.4(2) . . . . ? S6 Ru2 S5 C10 92.3(2) . . . . ? Cl3 Ru2 S5 C10 57(8) . . . . ? Cl4 Ru2 S5 C10 0.9(2) . . . . ? N2 Ru2 S5 C9 25.5(2) . . . . ? S4 Ru2 S5 C9 -61.1(2) . . . . ? S6 Ru2 S5 C9 -157.4(2) . . . . ? Cl3 Ru2 S5 C9 167(39) . . . . ? Cl4 Ru2 S5 C9 111.1(2) . . . . ? N2 Ru2 S6 O6 -121.7(13) . . . . ? S4 Ru2 S6 O6 6.91(17) . . . . ? S5 Ru2 S6 O6 97.25(17) . . . . ? Cl3 Ru2 S6 O6 -83.00(17) . . . . ? Cl4 Ru2 S6 O6 -170.46(17) . . . . ? N2 Ru2 S6 C11 110.5(13) . . . . ? S4 Ru2 S6 C11 -120.9(2) . . . . ? S5 Ru2 S6 C11 -30.6(2) . . . . ? Cl3 Ru2 S6 C11 149.1(2) . . . . ? Cl4 Ru2 S6 C11 61.7(2) . . . . ? N2 Ru2 S6 C12 1.7(14) . . . . ? S4 Ru2 S6 C12 130.27(19) . . . . ? S5 Ru2 S6 C12 -139.39(19) . . . . ? Cl3 Ru2 S6 C12 40.36(19) . . . . ? Cl4 Ru2 S6 C12 -47.1(2) . . . . ? S1 Ru1 N1 C13 -179.7(3) . . . . ? S2 Ru1 N1 C13 -90.0(3) . . . . ? S3 Ru1 N1 C13 37.0(13) . . . . ? Cl1 Ru1 N1 C13 87.7(3) . . . . ? Cl2 Ru1 N1 C13 -0.3(3) . . . . ? S4 Ru2 N2 C14 -88.8(3) . . . . ? S5 Ru2 N2 C14 -178.7(3) . . . . ? S6 Ru2 N2 C14 40.1(15) . . . . ? Cl3 Ru2 N2 C14 1.5(3) . . . . ? Cl4 Ru2 N2 C14 89.0(3) . . . . ? Ru1 N1 C13 C14 175.6(3) . . . . ? Ru2 N2 C14 C13 174.1(3) . . . . ? N1 C13 C14 N2 -77.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.338 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.110 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 828781' #TrackingRef '- Alessio- Bratsos CIF files.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H26 Cl F6 N2 O3 P Ru S3' _chemical_formula_weight 575.98 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 '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' H H 0.0000 0.0000 '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 9.2800(8) _cell_length_b 16.9870(11) _cell_length_c 12.5940(15) _cell_angle_alpha 90.00 _cell_angle_beta 92.718(10) _cell_angle_gamma 90.00 _cell_volume 1983.1(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 needle _exptl_crystal_colour 'pale 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 1.929 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.387 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6475 _exptl_absorpt_correction_T_max 0.7475 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Quadratic fit to sin(theta)/lambda - 18 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 22094 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 28.00 _reflns_number_total 4605 _reflns_number_gt 2779 _reflns_threshold_expression >2\s(I) _computing_data_collection 'XPRESS (MacScience, 2002)' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX97 (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^)+(0.0480P)^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 4605 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1019 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 0.861 _refine_ls_restrained_S_all 0.861 _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 0.76229(4) 0.17066(2) 0.17418(2) 0.03976(11) Uani 1 1 d . . . Cl1 Cl 0.77847(13) 0.03036(6) 0.14512(9) 0.0538(3) Uani 1 1 d . . . S1 S 0.95140(12) 0.19584(7) 0.07038(9) 0.0469(3) Uani 1 1 d . . . S2 S 0.59630(12) 0.17856(7) 0.03395(8) 0.0476(3) Uani 1 1 d . . . S3 S 0.73822(13) 0.29942(7) 0.21942(8) 0.0471(3) Uani 1 1 d . . . O1 O 0.9264(3) 0.24735(19) -0.0230(2) 0.0568(8) Uani 1 1 d . . . O2 O 0.5321(4) 0.2560(2) 0.0071(3) 0.0734(11) Uani 1 1 d . . . O3 O 0.8256(4) 0.32074(18) 0.3169(2) 0.0657(10) Uani 1 1 d . . . N1 N 0.6058(4) 0.1370(2) 0.2872(3) 0.0507(9) Uani 1 1 d . . . H1C H 0.5314 0.1710 0.2837 0.061 Uiso 1 1 calc R . . H1D H 0.5715 0.0886 0.2712 0.061 Uiso 1 1 calc R . . N2 N 0.9002(4) 0.1524(2) 0.3143(3) 0.0472(9) Uani 1 1 d . . . H2C H 0.9790 0.1252 0.2970 0.057 Uiso 1 1 calc R . . H2D H 0.9293 0.1992 0.3409 0.057 Uiso 1 1 calc R . . C1 C 0.6740(5) 0.1370(3) 0.3960(4) 0.0649(14) Uani 1 1 d . . . H1A H 0.6727 0.1900 0.4247 0.078 Uiso 1 1 calc R . . H1B H 0.6191 0.1034 0.4414 0.078 Uiso 1 1 calc R . . C2 C 0.8237(5) 0.1087(3) 0.3954(4) 0.0605(13) Uani 1 1 d . . . H2A H 0.8248 0.0528 0.3795 0.073 Uiso 1 1 calc R . . H2B H 0.8713 0.1167 0.4648 0.073 Uiso 1 1 calc R . . C3 C 1.0994(5) 0.2374(3) 0.1472(4) 0.0637(13) Uani 1 1 d . . . H3A H 1.1786 0.2463 0.1023 0.095 Uiso 1 1 calc R . . H3B H 1.1289 0.2017 0.2032 0.095 Uiso 1 1 calc R . . H3C H 1.0703 0.2864 0.1774 0.095 Uiso 1 1 calc R . . C4 C 1.0386(5) 0.1103(3) 0.0235(4) 0.0636(13) Uani 1 1 d . . . H4A H 0.9721 0.0808 -0.0217 0.095 Uiso 1 1 calc R . . H4B H 1.0706 0.0783 0.0828 0.095 Uiso 1 1 calc R . . H4C H 1.1200 0.1255 -0.0160 0.095 Uiso 1 1 calc R . . C5 C 0.6558(6) 0.1378(4) -0.0855(4) 0.0716(16) Uani 1 1 d . . . H5A H 0.5759 0.1342 -0.1366 0.107 Uiso 1 1 calc R . . H5B H 0.6945 0.0862 -0.0718 0.107 Uiso 1 1 calc R . . H5C H 0.7291 0.1708 -0.1131 0.107 Uiso 1 1 calc R . . C6 C 0.4502(5) 0.1138(3) 0.0537(4) 0.0733(16) Uani 1 1 d . . . H6A H 0.3965 0.1322 0.1121 0.110 Uiso 1 1 calc R . . H6B H 0.4867 0.0619 0.0693 0.110 Uiso 1 1 calc R . . H6C H 0.3883 0.1121 -0.0095 0.110 Uiso 1 1 calc R . . C7 C 0.7758(6) 0.3713(3) 0.1219(4) 0.0690(15) Uani 1 1 d . . . H7A H 0.7581 0.4228 0.1496 0.104 Uiso 1 1 calc R . . H7B H 0.7147 0.3625 0.0594 0.104 Uiso 1 1 calc R . . H7C H 0.8750 0.3672 0.1042 0.104 Uiso 1 1 calc R . . C8 C 0.5572(5) 0.3274(3) 0.2432(4) 0.0642(14) Uani 1 1 d . . . H8A H 0.5235 0.2976 0.3019 0.096 Uiso 1 1 calc R . . H8B H 0.4967 0.3170 0.1808 0.096 Uiso 1 1 calc R . . H8C H 0.5542 0.3825 0.2597 0.096 Uiso 1 1 calc R . . P1 P 0.26041(14) 0.00493(8) 0.32453(9) 0.0562(3) Uani 1 1 d . . . F1 F 0.2636(4) 0.0976(2) 0.3033(3) 0.1072(12) Uani 1 1 d . . . F2 F 0.4032(4) -0.0044(2) 0.2615(3) 0.0947(11) Uani 1 1 d . . . F3 F 0.3524(5) 0.0168(2) 0.4296(3) 0.1141(14) Uani 1 1 d . . . F4 F 0.2569(4) -0.08708(18) 0.3431(2) 0.0863(10) Uani 1 1 d . . . F5 F 0.1167(4) 0.0146(2) 0.3857(4) 0.1227(14) Uani 1 1 d . . . F6 F 0.1677(4) -0.0074(3) 0.2174(3) 0.1192(15) 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 0.0428(2) 0.03691(19) 0.03940(17) 0.00081(14) 0.00039(14) 0.00130(16) Cl1 0.0647(7) 0.0371(6) 0.0593(7) -0.0034(5) -0.0005(6) 0.0025(5) S1 0.0462(6) 0.0475(7) 0.0473(6) 0.0041(5) 0.0053(5) -0.0002(5) S2 0.0496(6) 0.0488(7) 0.0438(6) -0.0014(5) -0.0049(5) 0.0035(5) S3 0.0569(7) 0.0383(6) 0.0458(6) -0.0017(4) -0.0026(5) 0.0059(5) O1 0.062(2) 0.054(2) 0.0554(17) 0.0143(15) 0.0087(15) 0.0004(16) O2 0.098(3) 0.055(2) 0.064(2) -0.0043(16) -0.030(2) 0.0235(19) O3 0.084(3) 0.051(2) 0.059(2) -0.0129(15) -0.0269(18) 0.0041(18) N1 0.047(2) 0.057(2) 0.048(2) 0.0030(17) 0.0053(17) -0.0007(18) N2 0.051(2) 0.043(2) 0.0472(19) 0.0031(15) 0.0012(17) 0.0032(17) C1 0.067(3) 0.080(4) 0.048(3) 0.012(2) 0.008(2) 0.010(3) C2 0.060(3) 0.069(4) 0.051(3) 0.014(2) -0.005(2) -0.009(3) C3 0.047(3) 0.074(4) 0.069(3) 0.003(3) -0.001(2) -0.012(3) C4 0.064(3) 0.062(3) 0.066(3) 0.002(2) 0.017(3) 0.015(3) C5 0.076(4) 0.092(4) 0.046(3) -0.019(3) -0.009(3) 0.008(3) C6 0.053(3) 0.087(4) 0.079(4) 0.014(3) -0.012(3) -0.013(3) C7 0.096(4) 0.047(3) 0.065(3) 0.008(2) 0.011(3) 0.004(3) C8 0.070(3) 0.064(3) 0.059(3) -0.009(2) 0.002(3) 0.022(3) P1 0.0573(8) 0.0574(8) 0.0540(7) 0.0063(6) 0.0037(6) 0.0066(6) F1 0.136(3) 0.057(2) 0.130(3) 0.0242(19) 0.025(2) 0.018(2) F2 0.086(2) 0.084(3) 0.118(3) -0.016(2) 0.042(2) -0.0166(19) F3 0.153(4) 0.108(3) 0.077(2) -0.015(2) -0.039(2) 0.014(3) F4 0.099(3) 0.061(2) 0.099(2) 0.0145(17) 0.0090(19) -0.0029(18) F5 0.098(3) 0.112(3) 0.163(4) 0.015(3) 0.062(3) 0.027(2) F6 0.114(3) 0.146(4) 0.094(3) 0.021(2) -0.039(2) -0.013(3) _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 2.153(3) . ? Ru N1 2.158(4) . ? Ru S3 2.2740(12) . ? Ru S1 2.2780(12) . ? Ru S2 2.2917(11) . ? Ru Cl1 2.4169(11) . ? S1 O1 1.476(3) . ? S1 C4 1.778(5) . ? S1 C3 1.787(4) . ? S2 O2 1.477(3) . ? S2 C5 1.769(5) . ? S2 C6 1.773(5) . ? S3 O3 1.483(3) . ? S3 C7 1.777(5) . ? S3 C8 1.784(5) . ? N1 C1 1.482(5) . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 C2 1.472(5) . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? C1 C2 1.471(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? P1 F3 1.553(3) . ? P1 F6 1.579(3) . ? P1 F5 1.580(4) . ? P1 F4 1.581(3) . ? P1 F2 1.585(4) . ? P1 F1 1.597(3) . ? 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 79.27(13) . . ? N2 Ru S3 89.71(10) . . ? N1 Ru S3 90.72(11) . . ? N2 Ru S1 93.06(10) . . ? N1 Ru S1 171.50(10) . . ? S3 Ru S1 92.91(4) . . ? N2 Ru S2 172.71(10) . . ? N1 Ru S2 94.29(9) . . ? S3 Ru S2 93.80(4) . . ? S1 Ru S2 93.13(4) . . ? N2 Ru Cl1 86.74(10) . . ? N1 Ru Cl1 83.51(11) . . ? S3 Ru Cl1 173.71(4) . . ? S1 Ru Cl1 92.47(4) . . ? S2 Ru Cl1 89.16(4) . . ? O1 S1 C4 106.1(2) . . ? O1 S1 C3 106.6(2) . . ? C4 S1 C3 98.8(3) . . ? O1 S1 Ru 118.19(14) . . ? C4 S1 Ru 114.34(18) . . ? C3 S1 Ru 110.90(17) . . ? O2 S2 C5 107.1(2) . . ? O2 S2 C6 106.4(2) . . ? C5 S2 C6 98.5(3) . . ? O2 S2 Ru 118.52(13) . . ? C5 S2 Ru 114.04(17) . . ? C6 S2 Ru 110.23(16) . . ? O3 S3 C7 106.6(2) . . ? O3 S3 C8 106.2(2) . . ? C7 S3 C8 98.7(3) . . ? O3 S3 Ru 112.69(13) . . ? C7 S3 Ru 117.55(19) . . ? C8 S3 Ru 113.73(18) . . ? C1 N1 Ru 109.8(3) . . ? C1 N1 H1C 109.7 . . ? Ru N1 H1C 109.7 . . ? C1 N1 H1D 109.7 . . ? Ru N1 H1D 109.7 . . ? H1C N1 H1D 108.2 . . ? C2 N2 Ru 110.7(3) . . ? C2 N2 H2C 109.5 . . ? Ru N2 H2C 109.5 . . ? C2 N2 H2D 109.5 . . ? Ru N2 H2D 109.5 . . ? H2C N2 H2D 108.1 . . ? C2 C1 N1 110.9(4) . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 108.0 . . ? C1 C2 N2 109.0(4) . . ? C1 C2 H2A 109.9 . . ? N2 C2 H2A 109.9 . . ? C1 C2 H2B 109.9 . . ? N2 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? S1 C3 H3A 109.5 . . ? S1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? S1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? S1 C4 H4A 109.5 . . ? S1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? S2 C5 H5A 109.5 . . ? S2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? S2 C6 H6A 109.5 . . ? S2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? S2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? S3 C7 H7A 109.5 . . ? S3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? S3 C8 H8A 109.5 . . ? S3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? F3 P1 F6 179.7(3) . . ? F3 P1 F5 90.8(3) . . ? F6 P1 F5 89.5(3) . . ? F3 P1 F4 90.95(18) . . ? F6 P1 F4 88.9(2) . . ? F5 P1 F4 90.4(2) . . ? F3 P1 F2 90.0(2) . . ? F6 P1 F2 89.6(2) . . ? F5 P1 F2 179.1(2) . . ? F4 P1 F2 89.94(19) . . ? F3 P1 F1 90.0(2) . . ? F6 P1 F1 90.1(2) . . ? F5 P1 F1 90.1(2) . . ? F4 P1 F1 178.9(2) . . ? F2 P1 F1 89.5(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 N2 Ru S1 O1 -152.24(18) . . . . ? N1 Ru S1 O1 -177.5(7) . . . . ? S3 Ru S1 O1 -62.38(16) . . . . ? S2 Ru S1 O1 31.59(16) . . . . ? Cl1 Ru S1 O1 120.89(16) . . . . ? N2 Ru S1 C4 81.8(2) . . . . ? N1 Ru S1 C4 56.5(7) . . . . ? S3 Ru S1 C4 171.68(18) . . . . ? S2 Ru S1 C4 -94.35(19) . . . . ? Cl1 Ru S1 C4 -5.05(18) . . . . ? N2 Ru S1 C3 -28.8(2) . . . . ? N1 Ru S1 C3 -54.1(7) . . . . ? S3 Ru S1 C3 61.08(19) . . . . ? S2 Ru S1 C3 155.06(19) . . . . ? Cl1 Ru S1 C3 -115.65(19) . . . . ? N2 Ru S2 O2 122.5(8) . . . . ? N1 Ru S2 O2 94.9(2) . . . . ? S3 Ru S2 O2 3.9(2) . . . . ? S1 Ru S2 O2 -89.3(2) . . . . ? Cl1 Ru S2 O2 178.3(2) . . . . ? N2 Ru S2 C5 -110.0(8) . . . . ? N1 Ru S2 C5 -137.7(2) . . . . ? S3 Ru S2 C5 131.3(2) . . . . ? S1 Ru S2 C5 38.2(2) . . . . ? Cl1 Ru S2 C5 -54.3(2) . . . . ? N2 Ru S2 C6 -0.3(9) . . . . ? N1 Ru S2 C6 -28.0(2) . . . . ? S3 Ru S2 C6 -119.0(2) . . . . ? S1 Ru S2 C6 147.9(2) . . . . ? Cl1 Ru S2 C6 55.4(2) . . . . ? N2 Ru S3 O3 2.8(2) . . . . ? N1 Ru S3 O3 82.1(2) . . . . ? S1 Ru S3 O3 -90.22(18) . . . . ? S2 Ru S3 O3 176.44(18) . . . . ? Cl1 Ru S3 O3 58.5(4) . . . . ? N2 Ru S3 C7 127.4(2) . . . . ? N1 Ru S3 C7 -153.3(2) . . . . ? S1 Ru S3 C7 34.4(2) . . . . ? S2 Ru S3 C7 -58.9(2) . . . . ? Cl1 Ru S3 C7 -176.9(4) . . . . ? N2 Ru S3 C8 -118.1(2) . . . . ? N1 Ru S3 C8 -38.8(2) . . . . ? S1 Ru S3 C8 148.89(18) . . . . ? S2 Ru S3 C8 55.55(19) . . . . ? Cl1 Ru S3 C8 -62.4(4) . . . . ? N2 Ru N1 C1 11.4(3) . . . . ? S3 Ru N1 C1 -78.1(3) . . . . ? S1 Ru N1 C1 37.2(9) . . . . ? S2 Ru N1 C1 -172.0(3) . . . . ? Cl1 Ru N1 C1 99.3(3) . . . . ? N1 Ru N2 C2 15.1(3) . . . . ? S3 Ru N2 C2 105.9(3) . . . . ? S1 Ru N2 C2 -161.2(3) . . . . ? S2 Ru N2 C2 -13.0(10) . . . . ? Cl1 Ru N2 C2 -68.9(3) . . . . ? Ru N1 C1 C2 -36.9(5) . . . . ? N1 C1 C2 N2 50.7(6) . . . . ? Ru N2 C2 C1 -39.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.505 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.098 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 828782' #TrackingRef '- Alessio- Bratsos CIF files.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C12 H32 Cl N2 O3 Ru S3 1+), 2(P F6 1-), C H2 Cl2' _chemical_formula_sum 'C25 H66 Cl4 F12 N4 O6 P2 Ru2 S6' _chemical_formula_weight 1345.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 21.399(4) _cell_length_b 16.056(3) _cell_length_c 15.126(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.37(2) _cell_angle_gamma 90.00 _cell_volume 5192.6(15) _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 Cube _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2728 _exptl_absorpt_coefficient_mu 1.173 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6202 _exptl_absorpt_correction_T_max 0.7361 _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 69933 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.1169 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 24.71 _reflns_number_total 8475 _reflns_number_gt 4060 _reflns_threshold_expression >2\s(I) _computing_data_collection 'XPRESS (MacScience, 2002)' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX97 (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^)+(0.0603P)^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 8475 _refine_ls_number_parameters 562 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1314 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 0.830 _refine_ls_restrained_S_all 0.830 _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 0.36690(3) 0.29535(4) 0.76985(3) 0.05626(19) Uani 1 1 d . . . Cl1 Cl 0.26362(9) 0.28618(12) 0.82634(12) 0.0723(5) Uani 1 1 d . . . S1 S 0.38425(9) 0.15639(12) 0.79486(12) 0.0682(6) Uani 1 1 d . . . S2 S 0.32532(9) 0.27502(12) 0.62967(11) 0.0647(5) Uani 1 1 d . . . S3 S 0.46728(9) 0.31520(13) 0.72876(12) 0.0660(5) Uani 1 1 d . . . O1 O 0.4006(3) 0.1052(3) 0.7178(3) 0.0885(17) Uani 1 1 d . . . O2 O 0.3692(2) 0.2729(3) 0.5560(3) 0.0743(15) Uani 1 1 d . . . O3 O 0.5115(2) 0.3278(3) 0.8060(3) 0.0787(15) Uani 1 1 d . . . N1 N 0.3489(3) 0.4271(3) 0.7662(3) 0.0598(15) Uani 1 1 d . . . H1A H 0.3624 0.4488 0.7155 0.072 Uiso 1 1 calc R . . H1B H 0.3076 0.4365 0.7683 0.072 Uiso 1 1 calc R . . N2 N 0.3984(3) 0.3282(4) 0.9003(3) 0.0635(16) Uani 1 1 d . . . H2A H 0.3832 0.2917 0.9391 0.076 Uiso 1 1 calc R . . H2B H 0.4404 0.3256 0.9047 0.076 Uiso 1 1 calc R . . C1 C 0.3823(4) 0.4674(5) 0.8434(4) 0.067(2) Uani 1 1 d . . . H1 H 0.4266 0.4710 0.8300 0.081 Uiso 1 1 calc R . . C2 C 0.3777(4) 0.4132(4) 0.9223(4) 0.066(2) Uani 1 1 d . . . H2 H 0.3335 0.4101 0.9369 0.079 Uiso 1 1 calc R . . C3 C 0.4141(4) 0.4486(5) 1.0024(4) 0.074(2) Uani 1 1 d . . . H3A H 0.4075 0.4137 1.0535 0.088 Uiso 1 1 calc R . . H3B H 0.4584 0.4482 0.9913 0.088 Uiso 1 1 calc R . . C4 C 0.3939(4) 0.5366(5) 1.0222(5) 0.094(3) Uani 1 1 d . . . H4A H 0.3519 0.5355 1.0438 0.113 Uiso 1 1 calc R . . H4B H 0.4214 0.5594 1.0687 0.113 Uiso 1 1 calc R . . C5 C 0.3949(4) 0.5927(5) 0.9425(5) 0.091(3) Uani 1 1 d . . . H5A H 0.4380 0.6028 0.9280 0.110 Uiso 1 1 calc R . . H5B H 0.3764 0.6459 0.9570 0.110 Uiso 1 1 calc R . . C6 C 0.3595(4) 0.5562(5) 0.8613(5) 0.076(2) Uani 1 1 d . . . H6A H 0.3662 0.5910 0.8101 0.091 Uiso 1 1 calc R . . H6B H 0.3151 0.5554 0.8713 0.091 Uiso 1 1 calc R . . C7 C 0.3222(4) 0.1046(5) 0.8471(5) 0.092(3) Uani 1 1 d . . . H7A H 0.3354 0.0496 0.8641 0.138 Uiso 1 1 calc R . . H7B H 0.2865 0.1011 0.8067 0.138 Uiso 1 1 calc R . . H7C H 0.3113 0.1353 0.8987 0.138 Uiso 1 1 calc R . . C8 C 0.4443(4) 0.1395(5) 0.8782(5) 0.084(2) Uani 1 1 d . . . H8A H 0.4795 0.1743 0.8668 0.126 Uiso 1 1 calc R . . H8B H 0.4569 0.0822 0.8776 0.126 Uiso 1 1 calc R . . H8C H 0.4288 0.1531 0.9351 0.126 Uiso 1 1 calc R . . C9 C 0.2765(4) 0.1849(5) 0.6176(5) 0.084(2) Uani 1 1 d . . . H9A H 0.3014 0.1357 0.6258 0.125 Uiso 1 1 calc R . . H9B H 0.2567 0.1844 0.5594 0.125 Uiso 1 1 calc R . . H9C H 0.2450 0.1864 0.6610 0.125 Uiso 1 1 calc R . . C10 C 0.2679(3) 0.3523(5) 0.6013(5) 0.084(3) Uani 1 1 d . . . H10A H 0.2444 0.3355 0.5488 0.127 Uiso 1 1 calc R . . H10B H 0.2882 0.4045 0.5906 0.127 Uiso 1 1 calc R . . H10C H 0.2401 0.3587 0.6490 0.127 Uiso 1 1 calc R . . C11 C 0.5011(4) 0.2363(5) 0.6632(5) 0.088(3) Uani 1 1 d . . . H11A H 0.5028 0.1850 0.6958 0.132 Uiso 1 1 calc R . . H11B H 0.5426 0.2526 0.6489 0.132 Uiso 1 1 calc R . . H11C H 0.4760 0.2288 0.6097 0.132 Uiso 1 1 calc R . . C12 C 0.4775(4) 0.3994(5) 0.6574(5) 0.086(3) Uani 1 1 d . . . H12A H 0.5207 0.4029 0.6428 0.129 Uiso 1 1 calc R . . H12B H 0.4654 0.4500 0.6860 0.129 Uiso 1 1 calc R . . H12C H 0.4520 0.3916 0.6043 0.129 Uiso 1 1 calc R . . Ru2 Ru 0.08473(3) 0.58282(4) 0.80368(4) 0.0601(2) Uani 1 1 d . . . Cl2 Cl 0.06530(10) 0.71083(12) 0.72310(13) 0.0830(6) Uani 1 1 d . . . S4 S 0.13469(11) 0.65101(13) 0.91872(12) 0.0729(6) Uani 1 1 d . . . S5 S 0.17481(10) 0.56651(13) 0.72919(12) 0.0702(6) Uani 1 1 d . . . S6 S 0.09350(9) 0.45960(11) 0.87878(11) 0.0629(5) Uani 1 1 d . . . O4 O 0.1990(3) 0.6236(4) 0.9424(3) 0.0918(16) Uani 1 1 d . . . O5 O 0.2141(2) 0.4916(3) 0.7479(3) 0.0793(15) Uani 1 1 d . . . O6 O 0.0445(2) 0.4518(3) 0.9457(3) 0.0734(15) Uani 1 1 d . . . N3 N 0.0272(3) 0.5268(4) 0.6986(3) 0.0713(17) Uani 1 1 d . . . H3C H 0.0247 0.5610 0.6514 0.086 Uiso 1 1 calc R . . H3D H 0.0442 0.4783 0.6818 0.086 Uiso 1 1 calc R . . N4 N -0.0063(3) 0.5992(4) 0.8555(4) 0.0673(17) Uani 1 1 d . . . H4C H -0.0095 0.5682 0.9047 0.081 Uiso 1 1 calc R . . H4D H -0.0118 0.6529 0.8699 0.081 Uiso 1 1 calc R . . C13 C -0.0352(4) 0.5119(6) 0.7308(6) 0.099(3) Uani 1 1 d . . . H13 H -0.0292 0.4633 0.7694 0.119 Uiso 1 1 calc R . . C14 C -0.0547(4) 0.5736(6) 0.7884(5) 0.093(3) Uani 1 1 d . . . H14 H -0.0583 0.6226 0.7500 0.111 Uiso 1 1 calc R . . C15 C -0.1189(4) 0.5665(5) 0.8229(5) 0.080(2) Uani 1 1 d . . . H15A H -0.1179 0.5277 0.8721 0.096 Uiso 1 1 calc R . . H15B H -0.1314 0.6204 0.8452 0.096 Uiso 1 1 calc R . . C16 C -0.1661(4) 0.5383(7) 0.7561(7) 0.118(4) Uani 1 1 d . . . H16A H -0.1794 0.5860 0.7208 0.142 Uiso 1 1 calc R . . H16B H -0.2023 0.5187 0.7866 0.142 Uiso 1 1 calc R . . C17 C -0.1466(4) 0.4719(7) 0.6957(7) 0.128(4) Uani 1 1 d . . . H17A H -0.1762 0.4698 0.6454 0.153 Uiso 1 1 calc R . . H17B H -0.1486 0.4189 0.7262 0.153 Uiso 1 1 calc R . . C18 C -0.0822(4) 0.4823(5) 0.6622(5) 0.080(2) Uani 1 1 d . . . H18A H -0.0684 0.4293 0.6392 0.096 Uiso 1 1 calc R . . H18B H -0.0839 0.5218 0.6136 0.096 Uiso 1 1 calc R . . C19 C 0.0914(4) 0.6467(5) 1.0180(4) 0.087(3) Uani 1 1 d . . . H19A H 0.1131 0.6776 1.0640 0.131 Uiso 1 1 calc R . . H19B H 0.0872 0.5897 1.0362 0.131 Uiso 1 1 calc R . . H19C H 0.0506 0.6703 1.0068 0.131 Uiso 1 1 calc R . . C20 C 0.1377(5) 0.7618(5) 0.9084(6) 0.105(3) Uani 1 1 d . . . H20A H 0.1698 0.7767 0.8688 0.158 Uiso 1 1 calc R . . H20B H 0.1469 0.7861 0.9654 0.158 Uiso 1 1 calc R . . H20C H 0.0981 0.7820 0.8854 0.158 Uiso 1 1 calc R . . C21 C 0.2242(4) 0.6546(5) 0.7359(6) 0.090(3) Uani 1 1 d . . . H21A H 0.2582 0.6472 0.6972 0.136 Uiso 1 1 calc R . . H21B H 0.2405 0.6610 0.7957 0.136 Uiso 1 1 calc R . . H21C H 0.2008 0.7034 0.7186 0.136 Uiso 1 1 calc R . . C22 C 0.1583(4) 0.5670(5) 0.6118(4) 0.092(3) Uani 1 1 d . . . H22A H 0.1360 0.5172 0.5950 0.138 Uiso 1 1 calc R . . H22B H 0.1968 0.5693 0.5815 0.138 Uiso 1 1 calc R . . H22C H 0.1332 0.6147 0.5961 0.138 Uiso 1 1 calc R . . C23 C 0.0894(4) 0.3694(4) 0.8105(5) 0.088(3) Uani 1 1 d . . . H23A H 0.0505 0.3694 0.7763 0.132 Uiso 1 1 calc R . . H23B H 0.0917 0.3204 0.8469 0.132 Uiso 1 1 calc R . . H23C H 0.1236 0.3696 0.7714 0.132 Uiso 1 1 calc R . . C24 C 0.1670(3) 0.4381(5) 0.9348(4) 0.078(2) Uani 1 1 d . . . H24A H 0.1648 0.3855 0.9648 0.118 Uiso 1 1 calc R . . H24B H 0.1765 0.4813 0.9771 0.118 Uiso 1 1 calc R . . H24C H 0.1992 0.4358 0.8925 0.118 Uiso 1 1 calc R . . P1 P 0.37328(15) 0.5973(2) 0.54577(18) 0.1070(9) Uani 1 1 d . . . F1 F 0.3424(5) 0.5246(8) 0.5875(7) 0.352(8) Uani 1 1 d . . . F2 F 0.4010(5) 0.6092(7) 0.6383(4) 0.266(5) Uani 1 1 d . . . F3 F 0.4333(6) 0.5458(6) 0.5313(7) 0.258(5) Uani 1 1 d . . . F4 F 0.4095(4) 0.6703(5) 0.5123(5) 0.200(3) Uani 1 1 d . . . F5 F 0.3559(6) 0.5712(6) 0.4535(5) 0.273(6) Uani 1 1 d . . . P2 P 0.07398(13) 0.31903(16) 0.53290(15) 0.0856(7) Uani 1 1 d . . . F6 F 0.3172(4) 0.6470(8) 0.5511(8) 0.297(6) Uani 1 1 d . . . F7 F 0.0238(3) 0.2973(5) 0.6038(5) 0.179(3) Uani 1 1 d . . . F8 F 0.0937(6) 0.3853(7) 0.5889(7) 0.286(7) Uani 1 1 d . . . F9 F 0.1209(4) 0.2622(7) 0.5732(10) 0.304(7) Uani 1 1 d . . . F10 F 0.1192(4) 0.3413(5) 0.4651(5) 0.241(5) Uani 1 1 d . . . F11 F 0.0490(6) 0.2438(8) 0.4930(8) 0.313(7) Uani 1 1 d . . . F12 F 0.0259(4) 0.3744(8) 0.4902(7) 0.264(6) Uani 1 1 d . . . C25 C 0.3352(6) 0.6675(11) 0.1956(8) 0.215(8) Uani 1 1 d . . . H25A H 0.3641 0.6215 0.1897 0.258 Uiso 1 1 calc R . . H25B H 0.3550 0.7168 0.1725 0.258 Uiso 1 1 calc R . . Cl3 Cl 0.26810(17) 0.6464(3) 0.1291(3) 0.212(2) Uani 1 1 d . . . Cl4 Cl 0.3255(2) 0.6817(3) 0.2975(2) 0.221(2) 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 0.0526(4) 0.0646(4) 0.0520(3) 0.0001(3) 0.0082(3) 0.0019(3) Cl1 0.0567(12) 0.0821(14) 0.0796(12) 0.0020(10) 0.0213(10) -0.0015(11) S1 0.0715(14) 0.0652(13) 0.0683(11) 0.0011(10) 0.0067(10) 0.0030(11) S2 0.0622(13) 0.0747(14) 0.0575(10) -0.0027(9) 0.0059(9) -0.0019(11) S3 0.0517(12) 0.0812(14) 0.0659(11) -0.0020(10) 0.0129(10) -0.0003(11) O1 0.116(5) 0.074(4) 0.076(3) -0.015(3) 0.014(3) 0.012(3) O2 0.078(4) 0.093(4) 0.052(3) -0.008(2) 0.008(3) -0.008(3) O3 0.051(3) 0.114(4) 0.071(3) -0.006(3) -0.001(3) -0.001(3) N1 0.058(4) 0.071(4) 0.050(3) -0.002(3) 0.009(3) 0.003(3) N2 0.064(4) 0.075(4) 0.052(3) 0.003(3) 0.006(3) 0.003(3) C1 0.063(5) 0.074(6) 0.065(4) 0.006(4) 0.007(4) -0.011(4) C2 0.083(6) 0.063(5) 0.053(4) -0.003(4) 0.014(4) 0.010(4) C3 0.089(6) 0.073(6) 0.059(4) 0.004(4) -0.003(4) -0.013(5) C4 0.123(8) 0.082(7) 0.077(5) -0.016(5) -0.003(5) -0.006(6) C5 0.113(8) 0.068(6) 0.093(6) -0.016(5) 0.009(6) -0.008(5) C6 0.078(6) 0.064(6) 0.086(5) -0.003(4) 0.006(5) 0.003(5) C7 0.084(6) 0.078(6) 0.116(7) 0.018(5) 0.014(5) -0.013(5) C8 0.080(6) 0.089(6) 0.083(5) 0.005(5) -0.004(5) 0.027(5) C9 0.089(6) 0.084(6) 0.076(5) -0.012(4) -0.010(4) -0.026(5) C10 0.066(6) 0.116(7) 0.070(5) 0.001(5) -0.011(4) 0.018(5) C11 0.073(6) 0.102(7) 0.091(6) -0.019(5) 0.028(5) 0.009(5) C12 0.081(6) 0.090(6) 0.090(6) 0.005(5) 0.035(5) -0.006(5) Ru2 0.0605(4) 0.0581(4) 0.0619(4) 0.0030(3) 0.0037(3) 0.0043(3) Cl2 0.0882(16) 0.0670(14) 0.0932(13) 0.0178(11) -0.0063(12) 0.0034(12) S4 0.0770(16) 0.0656(14) 0.0753(12) -0.0048(10) -0.0058(11) 0.0050(12) S5 0.0658(14) 0.0729(14) 0.0728(12) 0.0068(10) 0.0139(10) -0.0040(12) S6 0.0673(13) 0.0591(12) 0.0630(11) 0.0045(9) 0.0107(10) 0.0076(10) O4 0.066(4) 0.098(4) 0.109(4) -0.003(3) -0.023(3) 0.010(3) O5 0.068(4) 0.082(4) 0.089(3) 0.013(3) 0.018(3) 0.018(3) O6 0.072(4) 0.077(4) 0.074(3) 0.011(3) 0.025(3) 0.015(3) N3 0.063(4) 0.082(5) 0.069(4) -0.003(3) 0.007(3) 0.007(4) N4 0.066(4) 0.066(4) 0.070(4) 0.002(3) 0.010(3) 0.018(3) C13 0.074(6) 0.129(8) 0.097(6) -0.048(6) 0.019(5) -0.020(6) C14 0.055(6) 0.135(8) 0.087(6) -0.027(6) -0.008(5) 0.008(6) C15 0.058(5) 0.091(6) 0.091(6) -0.001(5) -0.001(5) 0.014(5) C16 0.059(6) 0.147(10) 0.149(9) -0.037(8) 0.008(6) 0.003(6) C17 0.081(8) 0.145(10) 0.157(9) -0.064(8) 0.006(7) -0.007(7) C18 0.073(6) 0.077(6) 0.091(6) -0.007(5) -0.003(5) 0.005(5) C19 0.105(7) 0.096(7) 0.063(4) -0.012(4) 0.013(5) 0.003(5) C20 0.127(9) 0.059(6) 0.128(7) -0.016(5) -0.008(6) -0.005(6) C21 0.075(6) 0.077(6) 0.120(7) 0.003(5) 0.022(5) -0.009(5) C22 0.099(7) 0.110(7) 0.067(5) 0.008(5) 0.015(5) 0.006(6) C23 0.126(8) 0.055(5) 0.082(5) -0.006(4) 0.009(5) 0.018(5) C24 0.079(6) 0.084(6) 0.072(5) 0.023(4) 0.009(4) 0.019(5) P1 0.108(2) 0.124(3) 0.0910(19) 0.0179(17) 0.0230(17) -0.020(2) F1 0.299(12) 0.410(15) 0.332(11) 0.281(12) -0.160(10) -0.262(12) F2 0.280(11) 0.432(15) 0.086(4) -0.004(6) -0.005(6) -0.137(11) F3 0.307(13) 0.221(10) 0.250(11) 0.012(8) 0.072(10) 0.082(10) F4 0.236(9) 0.156(7) 0.212(7) 0.045(6) 0.046(6) -0.056(6) F5 0.442(17) 0.203(9) 0.163(7) -0.028(6) -0.117(9) -0.034(10) P2 0.106(2) 0.0726(17) 0.0779(14) -0.0078(13) 0.0034(15) -0.0033(16) F6 0.149(8) 0.339(14) 0.408(16) 0.080(13) 0.089(10) 0.107(9) F7 0.157(6) 0.202(7) 0.184(6) 0.061(5) 0.062(5) -0.016(5) F8 0.343(14) 0.274(12) 0.250(9) -0.176(10) 0.113(10) -0.167(11) F9 0.118(6) 0.267(11) 0.525(19) 0.244(13) -0.013(9) 0.017(7) F10 0.288(10) 0.256(9) 0.193(7) 0.117(7) 0.170(7) 0.111(8) F11 0.282(13) 0.302(13) 0.360(14) -0.215(12) 0.077(12) -0.118(11) F12 0.185(8) 0.325(13) 0.283(10) 0.202(11) 0.030(8) 0.080(9) C25 0.118(10) 0.39(2) 0.137(10) -0.127(13) -0.031(8) 0.046(13) Cl3 0.111(3) 0.257(5) 0.262(4) -0.131(4) -0.038(3) 0.033(3) Cl4 0.194(4) 0.329(6) 0.139(3) 0.046(3) -0.015(3) 0.051(4) _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 Ru1 N2 2.125(5) . ? Ru1 N1 2.150(5) . ? Ru1 S3 2.2829(19) . ? Ru1 S2 2.2887(19) . ? Ru1 S1 2.291(2) . ? Ru1 Cl1 2.4069(18) . ? S1 O1 1.480(5) . ? S1 C7 1.779(7) . ? S1 C8 1.783(7) . ? S2 O2 1.487(4) . ? S2 C10 1.787(7) . ? S2 C9 1.789(7) . ? S3 O3 1.487(5) . ? S3 C12 1.750(7) . ? S3 C11 1.780(7) . ? N1 C1 1.491(8) . ? N2 C2 1.477(8) . ? C1 C2 1.485(9) . ? C1 C6 1.534(9) . ? C2 C3 1.523(10) . ? C3 C4 1.511(10) . ? C4 C5 1.506(10) . ? C5 C6 1.532(10) . ? Ru2 N4 2.145(5) . ? Ru2 N3 2.166(6) . ? Ru2 S4 2.284(2) . ? Ru2 S6 2.2853(19) . ? Ru2 S5 2.288(2) . ? Ru2 Cl2 2.417(2) . ? S4 O4 1.475(5) . ? S4 C20 1.787(8) . ? S4 C19 1.798(6) . ? S5 O5 1.489(5) . ? S5 C21 1.766(8) . ? S5 C22 1.796(7) . ? S6 O6 1.493(4) . ? S6 C23 1.779(7) . ? S6 C24 1.789(8) . ? N3 C13 1.459(9) . ? N4 C14 1.478(9) . ? C13 C14 1.394(10) . ? C13 C18 1.492(11) . ? C14 C15 1.494(10) . ? C15 C16 1.470(11) . ? C16 C17 1.476(11) . ? C17 C18 1.497(11) . ? P1 F6 1.446(8) . ? P1 F5 1.489(8) . ? P1 F1 1.494(7) . ? P1 F4 1.504(7) . ? P1 F2 1.509(7) . ? P1 F3 1.550(10) . ? P2 F8 1.414(7) . ? P2 F11 1.444(9) . ? P2 F9 1.470(8) . ? P2 F10 1.482(6) . ? P2 F12 1.486(8) . ? P2 F7 1.587(6) . ? C25 Cl4 1.581(10) . ? C25 Cl3 1.752(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru1 N1 80.2(2) . . ? N2 Ru1 S3 87.27(15) . . ? N1 Ru1 S3 91.43(15) . . ? N2 Ru1 S2 172.69(16) . . ? N1 Ru1 S2 93.12(15) . . ? S3 Ru1 S2 95.85(7) . . ? N2 Ru1 S1 92.59(16) . . ? N1 Ru1 S1 171.88(13) . . ? S3 Ru1 S1 91.89(7) . . ? S2 Ru1 S1 93.91(7) . . ? N2 Ru1 Cl1 86.91(15) . . ? N1 Ru1 Cl1 84.46(15) . . ? S3 Ru1 Cl1 173.37(7) . . ? S2 Ru1 Cl1 89.58(7) . . ? S1 Ru1 Cl1 91.53(7) . . ? O1 S1 C7 107.2(4) . . ? O1 S1 C8 106.6(3) . . ? C7 S1 C8 98.3(4) . . ? O1 S1 Ru1 116.9(2) . . ? C7 S1 Ru1 114.2(3) . . ? C8 S1 Ru1 111.8(3) . . ? O2 S2 C10 106.6(3) . . ? O2 S2 C9 106.8(3) . . ? C10 S2 C9 98.3(4) . . ? O2 S2 Ru1 117.7(2) . . ? C10 S2 Ru1 111.2(3) . . ? C9 S2 Ru1 114.4(3) . . ? O3 S3 C12 106.7(4) . . ? O3 S3 C11 105.9(4) . . ? C12 S3 C11 98.2(4) . . ? O3 S3 Ru1 112.35(19) . . ? C12 S3 Ru1 114.8(3) . . ? C11 S3 Ru1 117.4(3) . . ? C1 N1 Ru1 109.2(4) . . ? C2 N2 Ru1 110.6(4) . . ? C2 C1 N1 109.2(6) . . ? C2 C1 C6 111.8(6) . . ? N1 C1 C6 113.4(6) . . ? N2 C2 C1 109.3(5) . . ? N2 C2 C3 112.1(6) . . ? C1 C2 C3 111.8(6) . . ? C4 C3 C2 111.5(7) . . ? C5 C4 C3 112.8(6) . . ? C4 C5 C6 112.9(7) . . ? C5 C6 C1 110.3(7) . . ? N4 Ru2 N3 79.7(2) . . ? N4 Ru2 S4 93.81(17) . . ? N3 Ru2 S4 172.93(16) . . ? N4 Ru2 S6 88.94(16) . . ? N3 Ru2 S6 92.16(17) . . ? S4 Ru2 S6 90.57(7) . . ? N4 Ru2 S5 171.93(17) . . ? N3 Ru2 S5 93.22(15) . . ? S4 Ru2 S5 93.02(8) . . ? S6 Ru2 S5 95.28(7) . . ? N4 Ru2 Cl2 86.58(16) . . ? N3 Ru2 Cl2 84.41(17) . . ? S4 Ru2 Cl2 92.40(8) . . ? S6 Ru2 Cl2 174.78(8) . . ? S5 Ru2 Cl2 88.84(7) . . ? O4 S4 C20 106.4(4) . . ? O4 S4 C19 107.1(4) . . ? C20 S4 C19 97.7(4) . . ? O4 S4 Ru2 116.4(2) . . ? C20 S4 Ru2 115.3(3) . . ? C19 S4 Ru2 112.1(3) . . ? O5 S5 C21 107.7(4) . . ? O5 S5 C22 106.1(3) . . ? C21 S5 C22 98.4(4) . . ? O5 S5 Ru2 118.68(19) . . ? C21 S5 Ru2 113.2(3) . . ? C22 S5 Ru2 110.5(3) . . ? O6 S6 C23 107.8(3) . . ? O6 S6 C24 106.9(3) . . ? C23 S6 C24 98.0(4) . . ? O6 S6 Ru2 111.3(2) . . ? C23 S6 Ru2 114.5(3) . . ? C24 S6 Ru2 117.1(3) . . ? C13 N3 Ru2 108.8(4) . . ? C14 N4 Ru2 109.7(4) . . ? C14 C13 N3 113.2(7) . . ? C14 C13 C18 116.8(8) . . ? N3 C13 C18 114.8(6) . . ? C13 C14 N4 114.0(7) . . ? C13 C14 C15 117.9(8) . . ? N4 C14 C15 114.3(6) . . ? C16 C15 C14 113.5(7) . . ? C15 C16 C17 116.3(8) . . ? C16 C17 C18 114.7(8) . . ? C13 C18 C17 113.8(7) . . ? F6 P1 F5 91.8(7) . . ? F6 P1 F1 91.5(7) . . ? F5 P1 F1 94.5(6) . . ? F6 P1 F4 91.6(6) . . ? F5 P1 F4 90.9(5) . . ? F1 P1 F4 173.6(6) . . ? F6 P1 F2 100.0(7) . . ? F5 P1 F2 167.8(7) . . ? F1 P1 F2 82.5(5) . . ? F4 P1 F2 91.5(5) . . ? F6 P1 F3 175.0(6) . . ? F5 P1 F3 83.9(6) . . ? F1 P1 F3 91.5(7) . . ? F4 P1 F3 85.8(5) . . ? F2 P1 F3 84.3(6) . . ? F8 P2 F11 167.7(7) . . ? F8 P2 F9 92.1(8) . . ? F11 P2 F9 83.6(8) . . ? F8 P2 F10 92.6(6) . . ? F11 P2 F10 98.8(6) . . ? F9 P2 F10 89.0(5) . . ? F8 P2 F12 89.7(7) . . ? F11 P2 F12 94.7(8) . . ? F9 P2 F12 178.2(9) . . ? F10 P2 F12 90.8(4) . . ? F8 P2 F7 87.3(5) . . ? F11 P2 F7 81.4(5) . . ? F9 P2 F7 93.0(5) . . ? F10 P2 F7 178.0(5) . . ? F12 P2 F7 87.1(4) . . ? Cl4 C25 Cl3 116.7(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru1 S1 O1 -150.1(3) . . . . ? N1 Ru1 S1 O1 -176.8(11) . . . . ? S3 Ru1 S1 O1 -62.7(3) . . . . ? S2 Ru1 S1 O1 33.3(3) . . . . ? Cl1 Ru1 S1 O1 122.9(3) . . . . ? N2 Ru1 S1 C7 83.6(4) . . . . ? N1 Ru1 S1 C7 56.9(12) . . . . ? S3 Ru1 S1 C7 171.0(3) . . . . ? S2 Ru1 S1 C7 -93.0(3) . . . . ? Cl1 Ru1 S1 C7 -3.4(3) . . . . ? N2 Ru1 S1 C8 -26.9(3) . . . . ? N1 Ru1 S1 C8 -53.6(12) . . . . ? S3 Ru1 S1 C8 60.5(3) . . . . ? S2 Ru1 S1 C8 156.5(3) . . . . ? Cl1 Ru1 S1 C8 -113.8(3) . . . . ? N2 Ru1 S2 O2 119.4(12) . . . . ? N1 Ru1 S2 O2 96.2(3) . . . . ? S3 Ru1 S2 O2 4.5(3) . . . . ? S1 Ru1 S2 O2 -87.8(2) . . . . ? Cl1 Ru1 S2 O2 -179.3(2) . . . . ? N2 Ru1 S2 C10 -3.8(13) . . . . ? N1 Ru1 S2 C10 -27.0(3) . . . . ? S3 Ru1 S2 C10 -118.8(3) . . . . ? S1 Ru1 S2 C10 148.9(3) . . . . ? Cl1 Ru1 S2 C10 57.4(3) . . . . ? N2 Ru1 S2 C9 -114.0(12) . . . . ? N1 Ru1 S2 C9 -137.2(3) . . . . ? S3 Ru1 S2 C9 131.1(3) . . . . ? S1 Ru1 S2 C9 38.8(3) . . . . ? Cl1 Ru1 S2 C9 -52.7(3) . . . . ? N2 Ru1 S3 O3 8.9(3) . . . . ? N1 Ru1 S3 O3 89.0(3) . . . . ? S2 Ru1 S3 O3 -177.7(3) . . . . ? S1 Ru1 S3 O3 -83.6(3) . . . . ? Cl1 Ru1 S3 O3 37.5(8) . . . . ? N2 Ru1 S3 C12 -113.2(3) . . . . ? N1 Ru1 S3 C12 -33.2(3) . . . . ? S2 Ru1 S3 C12 60.1(3) . . . . ? S1 Ru1 S3 C12 154.2(3) . . . . ? Cl1 Ru1 S3 C12 -84.7(7) . . . . ? N2 Ru1 S3 C11 132.1(4) . . . . ? N1 Ru1 S3 C11 -147.8(3) . . . . ? S2 Ru1 S3 C11 -54.5(3) . . . . ? S1 Ru1 S3 C11 39.6(3) . . . . ? Cl1 Ru1 S3 C11 160.7(7) . . . . ? N2 Ru1 N1 C1 14.3(4) . . . . ? S3 Ru1 N1 C1 -72.7(4) . . . . ? S2 Ru1 N1 C1 -168.7(4) . . . . ? S1 Ru1 N1 C1 41.4(14) . . . . ? Cl1 Ru1 N1 C1 102.1(4) . . . . ? N1 Ru1 N2 C2 13.2(4) . . . . ? S3 Ru1 N2 C2 105.1(4) . . . . ? S2 Ru1 N2 C2 -10.3(15) . . . . ? S1 Ru1 N2 C2 -163.1(4) . . . . ? Cl1 Ru1 N2 C2 -71.7(4) . . . . ? Ru1 N1 C1 C2 -39.5(6) . . . . ? Ru1 N1 C1 C6 -164.9(4) . . . . ? Ru1 N2 C2 C1 -38.8(7) . . . . ? Ru1 N2 C2 C3 -163.3(4) . . . . ? N1 C1 C2 N2 52.0(8) . . . . ? C6 C1 C2 N2 178.4(6) . . . . ? N1 C1 C2 C3 176.7(6) . . . . ? C6 C1 C2 C3 -56.9(9) . . . . ? N2 C2 C3 C4 178.1(6) . . . . ? C1 C2 C3 C4 54.9(8) . . . . ? C2 C3 C4 C5 -51.8(10) . . . . ? C3 C4 C5 C6 51.3(10) . . . . ? C4 C5 C6 C1 -51.7(9) . . . . ? C2 C1 C6 C5 54.8(9) . . . . ? N1 C1 C6 C5 178.8(6) . . . . ? N4 Ru2 S4 O4 149.5(3) . . . . ? N3 Ru2 S4 O4 173.3(13) . . . . ? S6 Ru2 S4 O4 60.6(3) . . . . ? S5 Ru2 S4 O4 -34.8(3) . . . . ? Cl2 Ru2 S4 O4 -123.7(3) . . . . ? N4 Ru2 S4 C20 -84.8(4) . . . . ? N3 Ru2 S4 C20 -61.0(14) . . . . ? S6 Ru2 S4 C20 -173.8(4) . . . . ? S5 Ru2 S4 C20 90.9(4) . . . . ? Cl2 Ru2 S4 C20 1.9(4) . . . . ? N4 Ru2 S4 C19 25.8(3) . . . . ? N3 Ru2 S4 C19 49.6(14) . . . . ? S6 Ru2 S4 C19 -63.2(3) . . . . ? S5 Ru2 S4 C19 -158.5(3) . . . . ? Cl2 Ru2 S4 C19 112.5(3) . . . . ? N4 Ru2 S5 O5 -123.9(12) . . . . ? N3 Ru2 S5 O5 -95.0(3) . . . . ? S4 Ru2 S5 O5 88.3(3) . . . . ? S6 Ru2 S5 O5 -2.5(3) . . . . ? Cl2 Ru2 S5 O5 -179.3(3) . . . . ? N4 Ru2 S5 C21 108.4(12) . . . . ? N3 Ru2 S5 C21 137.3(4) . . . . ? S4 Ru2 S5 C21 -39.4(3) . . . . ? S6 Ru2 S5 C21 -130.3(3) . . . . ? Cl2 Ru2 S5 C21 52.9(3) . . . . ? N4 Ru2 S5 C22 -1.0(12) . . . . ? N3 Ru2 S5 C22 27.9(3) . . . . ? S4 Ru2 S5 C22 -148.8(3) . . . . ? S6 Ru2 S5 C22 120.4(3) . . . . ? Cl2 Ru2 S5 C22 -56.4(3) . . . . ? N4 Ru2 S6 O6 -13.7(3) . . . . ? N3 Ru2 S6 O6 -93.4(3) . . . . ? S4 Ru2 S6 O6 80.1(2) . . . . ? S5 Ru2 S6 O6 173.2(2) . . . . ? Cl2 Ru2 S6 O6 -44.7(8) . . . . ? N4 Ru2 S6 C23 108.9(4) . . . . ? N3 Ru2 S6 C23 29.3(4) . . . . ? S4 Ru2 S6 C23 -157.3(3) . . . . ? S5 Ru2 S6 C23 -64.2(3) . . . . ? Cl2 Ru2 S6 C23 78.0(8) . . . . ? N4 Ru2 S6 C24 -137.2(3) . . . . ? N3 Ru2 S6 C24 143.2(3) . . . . ? S4 Ru2 S6 C24 -43.4(3) . . . . ? S5 Ru2 S6 C24 49.7(3) . . . . ? Cl2 Ru2 S6 C24 -168.1(8) . . . . ? N4 Ru2 N3 C13 -14.6(5) . . . . ? S4 Ru2 N3 C13 -38.8(16) . . . . ? S6 Ru2 N3 C13 73.9(5) . . . . ? S5 Ru2 N3 C13 169.3(5) . . . . ? Cl2 Ru2 N3 C13 -102.2(5) . . . . ? N3 Ru2 N4 C14 -6.6(5) . . . . ? S4 Ru2 N4 C14 170.5(5) . . . . ? S6 Ru2 N4 C14 -99.0(5) . . . . ? S5 Ru2 N4 C14 22.7(15) . . . . ? Cl2 Ru2 N4 C14 78.3(5) . . . . ? Ru2 N3 C13 C14 35.8(10) . . . . ? Ru2 N3 C13 C18 173.3(6) . . . . ? N3 C13 C14 N4 -44.2(12) . . . . ? C18 C13 C14 N4 179.2(7) . . . . ? N3 C13 C14 C15 177.7(7) . . . . ? C18 C13 C14 C15 41.1(13) . . . . ? Ru2 N4 C14 C13 29.0(10) . . . . ? Ru2 N4 C14 C15 168.7(6) . . . . ? C13 C14 C15 C16 -40.1(12) . . . . ? N4 C14 C15 C16 -178.1(8) . . . . ? C14 C15 C16 C17 40.3(13) . . . . ? C15 C16 C17 C18 -42.2(13) . . . . ? C14 C13 C18 C17 -40.9(12) . . . . ? N3 C13 C18 C17 -176.9(8) . . . . ? C16 C17 C18 C13 40.8(13) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.806 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.081 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 828784' #TrackingRef '- Alessio- Bratsos CIF files.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H24 Cl F6 N2 O3 P Ru S3' _chemical_formula_weight 549.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 orthorhombic _symmetry_space_group_name_H-M 'P bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8150(11) _cell_length_b 17.1720(15) _cell_length_c 20.8050(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3863.8(6) _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 block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 1.419 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7490 _exptl_absorpt_correction_T_max 0.8467 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Quadratic fit to sin(theta)/lambda - 18 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 40326 _diffrn_reflns_av_R_equivalents 0.1040 _diffrn_reflns_av_sigmaI/netI 0.1610 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.10 _reflns_number_total 3336 _reflns_number_gt 1299 _reflns_threshold_expression >2\s(I) _computing_data_collection 'XPRESS (MacScience, 2002)' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX97 (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^)+(0.0508P)^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 3336 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1355 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1023 _refine_ls_goodness_of_fit_ref 0.781 _refine_ls_restrained_S_all 0.781 _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 0.24334(7) 0.17645(4) 0.38222(3) 0.0459(2) Uani 1 1 d . . . Cl1 Cl 0.0949(2) 0.27743(14) 0.35708(10) 0.0615(7) Uani 1 1 d . . . S1 S 0.3734(2) 0.22203(15) 0.30416(9) 0.0519(7) Uani 1 1 d . . . S2 S 0.3327(2) 0.24925(14) 0.46213(10) 0.0538(7) Uani 1 1 d . . . S3 S 0.3601(2) 0.07025(15) 0.40698(11) 0.0602(7) Uani 1 1 d . . . O1 O 0.4898(6) 0.1781(4) 0.2942(3) 0.0729(19) Uani 1 1 d . . . O2 O 0.4688(5) 0.2596(4) 0.4603(2) 0.0624(18) Uani 1 1 d . . . O3 O 0.3063(7) 0.0226(4) 0.4585(3) 0.097(3) Uani 1 1 d . . . C1 C 0.2990(9) 0.2261(6) 0.2278(3) 0.078(3) Uani 1 1 d . . . H1A H 0.3464 0.2583 0.1993 0.116 Uiso 1 1 calc R . . H1B H 0.2177 0.2476 0.2328 0.116 Uiso 1 1 calc R . . H1C H 0.2930 0.1745 0.2103 0.116 Uiso 1 1 calc R . . C2 C 0.4130(10) 0.3205(5) 0.3121(4) 0.080(3) Uani 1 1 d . . . H2A H 0.4700 0.3266 0.3472 0.120 Uiso 1 1 calc R . . H2B H 0.3399 0.3505 0.3205 0.120 Uiso 1 1 calc R . . H2C H 0.4509 0.3384 0.2731 0.120 Uiso 1 1 calc R . . C3 C 0.2697(10) 0.3453(5) 0.4690(4) 0.088(4) Uani 1 1 d . . . H3A H 0.2984 0.3689 0.5081 0.131 Uiso 1 1 calc R . . H3B H 0.1811 0.3424 0.4696 0.131 Uiso 1 1 calc R . . H3C H 0.2958 0.3761 0.4330 0.131 Uiso 1 1 calc R . . C4 C 0.2965(9) 0.2130(6) 0.5403(3) 0.081(3) Uani 1 1 d . . . H4A H 0.3001 0.1572 0.5400 0.121 Uiso 1 1 calc R . . H4B H 0.2147 0.2295 0.5521 0.121 Uiso 1 1 calc R . . H4C H 0.3551 0.2329 0.5708 0.121 Uiso 1 1 calc R . . C5 C 0.5142(9) 0.0876(6) 0.4284(5) 0.096(4) Uani 1 1 d . . . H5A H 0.5169 0.1220 0.4647 0.143 Uiso 1 1 calc R . . H5B H 0.5569 0.1110 0.3928 0.143 Uiso 1 1 calc R . . H5C H 0.5534 0.0392 0.4393 0.143 Uiso 1 1 calc R . . C6 C 0.3875(10) 0.0068(5) 0.3421(4) 0.078(3) Uani 1 1 d . . . H6A H 0.4378 -0.0360 0.3563 0.117 Uiso 1 1 calc R . . H6B H 0.4296 0.0344 0.3085 0.117 Uiso 1 1 calc R . . H6C H 0.3102 -0.0127 0.3262 0.117 Uiso 1 1 calc R . . N1 N 0.1063(7) 0.1309(4) 0.4475(3) 0.063(2) Uani 1 1 d . . . H1D H 0.0470 0.1072 0.4252 0.095 Uiso 1 1 calc R . . H1E H 0.0737 0.1698 0.4701 0.095 Uiso 1 1 calc R . . H1F H 0.1417 0.0969 0.4740 0.095 Uiso 1 1 calc R . . N2 N 0.1444(7) 0.1108(4) 0.3092(3) 0.057(2) Uani 1 1 d . . . H2D H 0.1003 0.0733 0.3278 0.085 Uiso 1 1 calc R . . H2E H 0.1983 0.0897 0.2820 0.085 Uiso 1 1 calc R . . H2F H 0.0940 0.1425 0.2878 0.085 Uiso 1 1 calc R . . P P -0.1650(3) -0.01963(19) 0.35486(14) 0.0786(10) Uani 1 1 d . . . F1 F -0.0508(8) -0.0114(5) 0.3126(4) 0.171(4) Uani 1 1 d . . . F2 F -0.2794(10) -0.0298(7) 0.3951(5) 0.233(6) Uani 1 1 d . . . F3 F -0.0841(11) -0.0555(7) 0.4052(4) 0.254(7) Uani 1 1 d . . . F4 F -0.1447(11) 0.0619(6) 0.3845(4) 0.207(5) Uani 1 1 d . . . F5 F -0.2471(9) 0.0195(5) 0.3049(3) 0.168(4) Uani 1 1 d . . . F6 F -0.1838(8) -0.0984(5) 0.3229(5) 0.206(5) 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 0.0494(5) 0.0446(4) 0.0439(4) -0.0013(4) -0.0001(4) -0.0003(4) Cl1 0.0618(18) 0.0538(16) 0.0689(14) 0.0001(12) -0.0050(12) 0.0124(14) S1 0.0528(18) 0.0546(17) 0.0483(13) 0.0026(11) 0.0055(11) -0.0051(14) S2 0.0577(18) 0.0567(17) 0.0469(13) -0.0038(12) -0.0039(12) -0.0016(14) S3 0.0698(19) 0.0524(17) 0.0584(14) 0.0033(13) 0.0036(13) 0.0092(15) O1 0.061(5) 0.082(5) 0.076(4) 0.023(4) 0.025(3) 0.018(4) O2 0.049(5) 0.068(5) 0.070(4) -0.001(3) -0.005(3) -0.007(4) O3 0.133(7) 0.070(5) 0.088(5) 0.036(4) 0.032(4) 0.014(5) C1 0.077(8) 0.114(10) 0.042(6) 0.018(5) -0.005(5) -0.011(7) C2 0.099(9) 0.069(8) 0.072(6) 0.006(6) 0.012(6) -0.033(7) C3 0.120(10) 0.064(7) 0.078(7) -0.038(5) -0.028(7) 0.032(7) C4 0.089(9) 0.122(9) 0.031(5) 0.004(5) -0.003(5) -0.017(7) C5 0.078(9) 0.071(9) 0.139(9) -0.006(7) -0.046(7) 0.028(7) C6 0.119(10) 0.037(6) 0.077(6) -0.016(5) -0.016(6) 0.023(6) N1 0.075(6) 0.059(6) 0.056(5) -0.005(4) 0.012(4) -0.001(5) N2 0.069(6) 0.054(5) 0.047(4) -0.003(4) 0.002(4) -0.010(4) P 0.095(3) 0.069(2) 0.0715(19) 0.0084(17) 0.018(2) 0.015(2) F1 0.150(8) 0.146(8) 0.217(8) 0.012(7) 0.098(7) -0.033(6) F2 0.236(12) 0.219(11) 0.244(10) 0.092(9) 0.163(10) 0.091(10) F3 0.294(15) 0.330(16) 0.139(7) 0.055(8) -0.030(8) 0.191(13) F4 0.222(11) 0.159(9) 0.241(10) -0.110(8) -0.070(8) 0.042(8) F5 0.217(9) 0.172(8) 0.114(5) 0.025(5) -0.042(6) 0.079(7) F6 0.121(7) 0.109(7) 0.388(14) -0.115(9) 0.032(8) -0.007(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 N1 2.157(6) . ? Ru N2 2.174(6) . ? Ru S3 2.277(3) . ? Ru S1 2.286(2) . ? Ru S2 2.294(2) . ? Ru Cl1 2.421(2) . ? S1 O1 1.482(6) . ? S1 C2 1.753(9) . ? S1 C1 1.781(8) . ? S2 O2 1.483(6) . ? S2 C4 1.784(8) . ? S2 C3 1.791(9) . ? S3 O3 1.469(6) . ? S3 C5 1.750(10) . ? S3 C6 1.760(8) . ? P F3 1.497(8) . ? P F2 1.505(9) . ? P F6 1.521(8) . ? P F1 1.522(7) . ? P F5 1.523(7) . ? P F4 1.546(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru N2 85.1(3) . . ? N1 Ru S3 87.0(2) . . ? N2 Ru S3 90.9(2) . . ? N1 Ru S1 173.68(19) . . ? N2 Ru S1 89.06(17) . . ? S3 Ru S1 95.37(10) . . ? N1 Ru S2 91.77(19) . . ? N2 Ru S2 175.4(2) . . ? S3 Ru S2 92.22(9) . . ? S1 Ru S2 93.96(9) . . ? N1 Ru Cl1 86.6(2) . . ? N2 Ru Cl1 83.9(2) . . ? S3 Ru Cl1 172.09(10) . . ? S1 Ru Cl1 90.53(9) . . ? S2 Ru Cl1 92.62(9) . . ? O1 S1 C2 107.2(5) . . ? O1 S1 C1 106.2(4) . . ? C2 S1 C1 99.0(5) . . ? O1 S1 Ru 116.6(3) . . ? C2 S1 Ru 114.4(3) . . ? C1 S1 Ru 111.7(3) . . ? O2 S2 C4 106.4(4) . . ? O2 S2 C3 105.6(5) . . ? C4 S2 C3 99.5(5) . . ? O2 S2 Ru 117.7(2) . . ? C4 S2 Ru 112.2(3) . . ? C3 S2 Ru 113.5(3) . . ? O3 S3 C5 106.7(5) . . ? O3 S3 C6 106.3(4) . . ? C5 S3 C6 98.1(5) . . ? O3 S3 Ru 113.0(3) . . ? C5 S3 Ru 116.7(4) . . ? C6 S3 Ru 114.6(3) . . ? F3 P F2 92.5(6) . . ? F3 P F6 91.1(7) . . ? F2 P F6 91.8(7) . . ? F3 P F1 88.2(6) . . ? F2 P F1 178.1(7) . . ? F6 P F1 86.5(5) . . ? F3 P F5 178.0(7) . . ? F2 P F5 87.2(6) . . ? F6 P F5 90.9(6) . . ? F1 P F5 92.1(5) . . ? F3 P F4 90.6(6) . . ? F2 P F4 89.9(6) . . ? F6 P F4 177.5(7) . . ? F1 P F4 91.8(6) . . ? F5 P F4 87.4(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ru S1 O1 -115.5(19) . . . . ? N2 Ru S1 O1 -94.1(4) . . . . ? S3 Ru S1 O1 -3.3(3) . . . . ? S2 Ru S1 O1 89.3(3) . . . . ? Cl1 Ru S1 O1 -178.0(3) . . . . ? N1 Ru S1 C2 118.3(19) . . . . ? N2 Ru S1 C2 139.7(5) . . . . ? S3 Ru S1 C2 -129.5(4) . . . . ? S2 Ru S1 C2 -36.9(4) . . . . ? Cl1 Ru S1 C2 55.8(4) . . . . ? N1 Ru S1 C1 6.8(19) . . . . ? N2 Ru S1 C1 28.2(4) . . . . ? S3 Ru S1 C1 119.0(4) . . . . ? S2 Ru S1 C1 -148.4(4) . . . . ? Cl1 Ru S1 C1 -55.7(4) . . . . ? N1 Ru S2 O2 145.2(4) . . . . ? N2 Ru S2 O2 -169(2) . . . . ? S3 Ru S2 O2 58.1(3) . . . . ? S1 Ru S2 O2 -37.4(3) . . . . ? Cl1 Ru S2 O2 -128.1(3) . . . . ? N1 Ru S2 C4 21.2(4) . . . . ? N2 Ru S2 C4 67(2) . . . . ? S3 Ru S2 C4 -65.9(4) . . . . ? S1 Ru S2 C4 -161.4(4) . . . . ? Cl1 Ru S2 C4 107.9(4) . . . . ? N1 Ru S2 C3 -90.6(5) . . . . ? N2 Ru S2 C3 -45(2) . . . . ? S3 Ru S2 C3 -177.7(4) . . . . ? S1 Ru S2 C3 86.7(4) . . . . ? Cl1 Ru S2 C3 -4.0(4) . . . . ? N1 Ru S3 O3 -6.2(4) . . . . ? N2 Ru S3 O3 -91.2(4) . . . . ? S1 Ru S3 O3 179.6(4) . . . . ? S2 Ru S3 O3 85.4(4) . . . . ? Cl1 Ru S3 O3 -42.3(7) . . . . ? N1 Ru S3 C5 -130.5(5) . . . . ? N2 Ru S3 C5 144.5(5) . . . . ? S1 Ru S3 C5 55.4(4) . . . . ? S2 Ru S3 C5 -38.8(4) . . . . ? Cl1 Ru S3 C5 -166.5(6) . . . . ? N1 Ru S3 C6 115.8(5) . . . . ? N2 Ru S3 C6 30.8(4) . . . . ? S1 Ru S3 C6 -58.3(4) . . . . ? S2 Ru S3 C6 -152.5(4) . . . . ? Cl1 Ru S3 C6 79.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.649 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.113 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 828786' #TrackingRef '- Alessio- Bratsos CIF files.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H22 Cl N O5 Ru S3' _chemical_formula_weight 493.01 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' 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' Cl Cl 0.1484 0.1585 '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 Tetragonal _symmetry_space_group_name_H-M 'P 42/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 21.307(4) _cell_length_b 21.307(4) _cell_length_c 7.959(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3613.3(13) _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 needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 1.383 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7638 _exptl_absorpt_correction_T_max 0.8375 _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 36298 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 29.63 _reflns_number_total 4966 _reflns_number_gt 3100 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XPRESS (MacScience, 2002)' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX97 (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^ > 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^)+(0.0308P)^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 4966 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0668 _refine_ls_wR_factor_gt 0.0631 _refine_ls_goodness_of_fit_ref 0.867 _refine_ls_restrained_S_all 0.867 _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 0.494851(10) 0.683303(9) 0.11731(2) 0.03289(6) Uani 1 1 d . . . Cl1 Cl 0.51489(4) 0.62438(3) -0.13807(7) 0.04784(17) Uani 1 1 d . . . N1 N 0.54960(10) 0.75385(10) -0.0007(2) 0.0380(5) Uani 1 1 d . . . O4 O 0.58541(9) 0.65715(9) 0.1888(2) 0.0446(4) Uani 1 1 d . . . O5 O 0.68583(11) 0.66936(11) 0.1157(3) 0.0668(6) Uani 1 1 d . . . C1 C 0.53022(14) 0.80278(13) -0.0938(3) 0.0428(6) Uani 1 1 d . . . H1 H 0.4874 0.8101 -0.1052 0.051 Uiso 1 1 calc R . . C2 C 0.57206(15) 0.84246(13) -0.1731(3) 0.0485(7) Uani 1 1 d . . . H2 H 0.5575 0.8760 -0.2368 0.058 Uiso 1 1 calc R . . C3 C 0.63498(16) 0.83192(15) -0.1570(3) 0.0548(8) Uani 1 1 d . . . H3 H 0.6638 0.8580 -0.2101 0.066 Uiso 1 1 calc R . . C4 C 0.65510(15) 0.78218(15) -0.0614(4) 0.0551(8) Uani 1 1 d . . . H4 H 0.6978 0.7750 -0.0469 0.066 Uiso 1 1 calc R . . C5 C 0.61159(13) 0.74263(13) 0.0135(3) 0.0424(6) Uani 1 1 d . . . C6 C 0.63089(15) 0.68576(14) 0.1132(3) 0.0473(7) Uani 1 1 d . . . S1 S 0.45717(3) 0.59095(3) 0.22469(8) 0.03939(15) Uani 1 1 d . . . S2 S 0.39824(3) 0.71549(3) 0.03021(8) 0.04009(16) Uani 1 1 d . . . S3 S 0.48480(3) 0.74147(3) 0.35227(7) 0.04173(16) Uani 1 1 d . . . O1 O 0.40523(10) 0.55964(9) 0.1343(2) 0.0518(5) Uani 1 1 d . . . O2 O 0.39039(10) 0.78439(9) 0.0171(3) 0.0555(5) Uani 1 1 d . . . O3 O 0.42529(10) 0.73730(10) 0.4467(2) 0.0556(5) Uani 1 1 d . . . C7 C 0.43526(15) 0.59003(14) 0.4409(3) 0.0516(8) Uani 1 1 d . . . H7A H 0.4003 0.6177 0.4580 0.077 Uiso 1 1 calc R . . H7B H 0.4701 0.6037 0.5082 0.077 Uiso 1 1 calc R . . H7C H 0.4236 0.5482 0.4728 0.077 Uiso 1 1 calc R . . C8 C 0.52093(14) 0.53768(13) 0.2310(4) 0.0549(8) Uani 1 1 d . . . H8A H 0.5066 0.4978 0.2722 0.082 Uiso 1 1 calc R . . H8B H 0.5529 0.5537 0.3043 0.082 Uiso 1 1 calc R . . H8C H 0.5378 0.5326 0.1200 0.082 Uiso 1 1 calc R . . C9 C 0.37588(15) 0.68337(16) -0.1667(4) 0.0604(9) Uani 1 1 d . . . H9A H 0.3331 0.6944 -0.1903 0.091 Uiso 1 1 calc R . . H9B H 0.3798 0.6385 -0.1630 0.091 Uiso 1 1 calc R . . H9C H 0.4026 0.6998 -0.2532 0.091 Uiso 1 1 calc R . . C10 C 0.33379(13) 0.68849(15) 0.1532(4) 0.0546(8) Uani 1 1 d . . . H10A H 0.3398 0.7007 0.2682 0.082 Uiso 1 1 calc R . . H10B H 0.3312 0.6436 0.1461 0.082 Uiso 1 1 calc R . . H10C H 0.2956 0.7067 0.1117 0.082 Uiso 1 1 calc R . . C11 C 0.49919(16) 0.82255(13) 0.3152(4) 0.0572(8) Uani 1 1 d . . . H11A H 0.4716 0.8374 0.2286 0.086 Uiso 1 1 calc R . . H11B H 0.5420 0.8282 0.2804 0.086 Uiso 1 1 calc R . . H11C H 0.4918 0.8458 0.4166 0.086 Uiso 1 1 calc R . . C12 C 0.54689(15) 0.72614(16) 0.4960(3) 0.0593(9) Uani 1 1 d . . . H12A H 0.5408 0.7505 0.5961 0.089 Uiso 1 1 calc R . . H12B H 0.5862 0.7373 0.4453 0.089 Uiso 1 1 calc R . . H12C H 0.5472 0.6823 0.5242 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.03512(13) 0.03132(12) 0.03222(11) 0.00114(8) 0.00117(8) -0.00013(9) Cl1 0.0582(5) 0.0439(4) 0.0414(3) -0.0065(3) 0.0071(3) 0.0022(3) N1 0.0396(14) 0.0373(13) 0.0372(11) -0.0026(9) 0.0037(9) -0.0013(10) O4 0.0385(12) 0.0434(12) 0.0519(11) 0.0054(8) -0.0034(8) 0.0014(9) O5 0.0412(14) 0.0641(16) 0.0950(17) 0.0071(12) 0.0032(12) 0.0092(11) C1 0.0451(17) 0.0385(17) 0.0449(15) 0.0037(11) 0.0013(11) -0.0022(12) C2 0.061(2) 0.0426(18) 0.0420(15) 0.0040(11) 0.0063(13) -0.0062(14) C3 0.058(2) 0.050(2) 0.0562(17) -0.0002(14) 0.0146(14) -0.0141(15) C4 0.0392(19) 0.055(2) 0.071(2) -0.0009(15) 0.0117(14) -0.0052(14) C5 0.0426(18) 0.0411(17) 0.0434(14) -0.0042(11) 0.0052(11) -0.0011(12) C6 0.0442(18) 0.0430(18) 0.0546(17) -0.0033(13) -0.0006(13) 0.0038(13) S1 0.0420(4) 0.0347(4) 0.0415(3) 0.0051(3) -0.0028(3) -0.0030(3) S2 0.0380(4) 0.0383(4) 0.0439(4) 0.0048(3) -0.0003(3) 0.0013(3) S3 0.0493(5) 0.0400(4) 0.0359(3) -0.0031(3) 0.0045(3) -0.0056(3) O1 0.0558(14) 0.0442(12) 0.0553(12) 0.0038(8) -0.0135(9) -0.0149(10) O2 0.0499(14) 0.0378(12) 0.0788(14) 0.0094(10) 0.0003(10) 0.0064(9) O3 0.0584(14) 0.0608(15) 0.0476(11) -0.0087(9) 0.0182(9) -0.0099(11) C7 0.058(2) 0.053(2) 0.0439(15) 0.0099(13) 0.0016(13) -0.0095(15) C8 0.056(2) 0.0387(18) 0.0702(19) 0.0104(14) -0.0030(15) 0.0092(14) C9 0.056(2) 0.073(2) 0.0524(17) 0.0004(15) -0.0140(14) -0.0014(17) C10 0.0351(17) 0.061(2) 0.0678(19) 0.0127(15) 0.0064(13) -0.0003(14) C11 0.077(2) 0.0376(18) 0.0566(18) -0.0103(13) 0.0148(15) -0.0058(15) C12 0.063(2) 0.073(2) 0.0412(16) -0.0006(14) -0.0090(13) -0.0171(17) _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 O4 2.0874(18) . ? Ru N1 2.122(2) . ? Ru S3 2.2537(8) . ? Ru S2 2.2778(8) . ? Ru S1 2.2907(8) . ? Ru Cl1 2.4269(8) . ? N1 C1 1.344(3) . ? N1 C5 1.347(3) . ? O4 C6 1.293(3) . ? O5 C6 1.222(3) . ? C1 C2 1.381(4) . ? C2 C3 1.365(4) . ? C3 C4 1.373(4) . ? C4 C5 1.387(4) . ? C5 C6 1.506(4) . ? S1 O1 1.4791(19) . ? S1 C8 1.771(3) . ? S1 C7 1.783(3) . ? S2 O2 1.481(2) . ? S2 C9 1.775(3) . ? S2 C10 1.782(3) . ? S3 O3 1.477(2) . ? S3 C12 1.779(3) . ? S3 C11 1.779(3) . ? 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 O4 Ru N1 78.56(8) . . ? O4 Ru S3 90.48(5) . . ? N1 Ru S3 91.72(6) . . ? O4 Ru S2 177.08(5) . . ? N1 Ru S2 98.56(6) . . ? S3 Ru S2 90.06(3) . . ? O4 Ru S1 89.60(5) . . ? N1 Ru S1 165.10(6) . . ? S3 Ru S1 97.44(3) . . ? S2 Ru S1 93.18(3) . . ? O4 Ru Cl1 85.85(5) . . ? N1 Ru Cl1 84.20(6) . . ? S3 Ru Cl1 174.98(3) . . ? S2 Ru Cl1 93.43(3) . . ? S1 Ru Cl1 85.97(3) . . ? C1 N1 C5 119.0(2) . . ? C1 N1 Ru 128.65(19) . . ? C5 N1 Ru 112.11(18) . . ? C6 O4 Ru 116.10(18) . . ? N1 C1 C2 121.9(3) . . ? C3 C2 C1 119.4(3) . . ? C2 C3 C4 119.0(3) . . ? C3 C4 C5 119.9(3) . . ? N1 C5 C4 120.8(3) . . ? N1 C5 C6 117.1(2) . . ? C4 C5 C6 122.2(3) . . ? O5 C6 O4 125.2(3) . . ? O5 C6 C5 120.0(3) . . ? O4 C6 C5 114.8(3) . . ? O1 S1 C8 107.38(14) . . ? O1 S1 C7 105.59(13) . . ? C8 S1 C7 99.58(15) . . ? O1 S1 Ru 117.92(8) . . ? C8 S1 Ru 106.99(10) . . ? C7 S1 Ru 117.47(10) . . ? O2 S2 C9 106.83(14) . . ? O2 S2 C10 105.77(14) . . ? C9 S2 C10 98.85(15) . . ? O2 S2 Ru 114.96(9) . . ? C9 S2 Ru 113.27(11) . . ? C10 S2 Ru 115.59(10) . . ? O3 S3 C12 107.46(14) . . ? O3 S3 C11 106.91(14) . . ? C12 S3 C11 99.02(15) . . ? O3 S3 Ru 118.09(9) . . ? C12 S3 Ru 111.22(11) . . ? C11 S3 Ru 112.33(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 O4 Ru N1 C1 -178.9(2) . . . . ? S3 Ru N1 C1 -88.8(2) . . . . ? S2 Ru N1 C1 1.6(2) . . . . ? S1 Ru N1 C1 143.2(2) . . . . ? Cl1 Ru N1 C1 94.2(2) . . . . ? O4 Ru N1 C5 6.67(16) . . . . ? S3 Ru N1 C5 96.81(16) . . . . ? S2 Ru N1 C5 -172.87(15) . . . . ? S1 Ru N1 C5 -31.3(3) . . . . ? Cl1 Ru N1 C5 -80.26(16) . . . . ? N1 Ru O4 C6 -10.85(19) . . . . ? S3 Ru O4 C6 -102.50(19) . . . . ? S2 Ru O4 C6 -1.9(12) . . . . ? S1 Ru O4 C6 160.06(19) . . . . ? Cl1 Ru O4 C6 74.07(19) . . . . ? C5 N1 C1 C2 -1.1(4) . . . . ? Ru N1 C1 C2 -175.16(19) . . . . ? N1 C1 C2 C3 0.0(4) . . . . ? C1 C2 C3 C4 -0.3(4) . . . . ? C2 C3 C4 C5 1.6(5) . . . . ? C1 N1 C5 C4 2.4(4) . . . . ? Ru N1 C5 C4 177.4(2) . . . . ? C1 N1 C5 C6 -177.5(2) . . . . ? Ru N1 C5 C6 -2.5(3) . . . . ? C3 C4 C5 N1 -2.7(4) . . . . ? C3 C4 C5 C6 177.2(3) . . . . ? Ru O4 C6 O5 -166.2(2) . . . . ? Ru O4 C6 C5 12.5(3) . . . . ? N1 C5 C6 O5 172.2(3) . . . . ? C4 C5 C6 O5 -7.7(4) . . . . ? N1 C5 C6 O4 -6.6(4) . . . . ? C4 C5 C6 O4 173.5(3) . . . . ? O4 Ru S1 O1 -143.16(11) . . . . ? N1 Ru S1 O1 -106.1(2) . . . . ? S3 Ru S1 O1 126.41(10) . . . . ? S2 Ru S1 O1 35.93(10) . . . . ? Cl1 Ru S1 O1 -57.29(10) . . . . ? O4 Ru S1 C8 -22.14(12) . . . . ? N1 Ru S1 C8 14.9(3) . . . . ? S3 Ru S1 C8 -112.57(11) . . . . ? S2 Ru S1 C8 156.95(11) . . . . ? Cl1 Ru S1 C8 63.73(11) . . . . ? O4 Ru S1 C7 88.65(13) . . . . ? N1 Ru S1 C7 125.7(2) . . . . ? S3 Ru S1 C7 -1.77(12) . . . . ? S2 Ru S1 C7 -92.25(12) . . . . ? Cl1 Ru S1 C7 174.53(12) . . . . ? O4 Ru S2 O2 -43.9(11) . . . . ? N1 Ru S2 O2 -35.03(11) . . . . ? S3 Ru S2 O2 56.71(9) . . . . ? S1 Ru S2 O2 154.17(9) . . . . ? Cl1 Ru S2 O2 -119.68(9) . . . . ? O4 Ru S2 C9 79.3(11) . . . . ? N1 Ru S2 C9 88.18(13) . . . . ? S3 Ru S2 C9 179.92(12) . . . . ? S1 Ru S2 C9 -82.62(12) . . . . ? Cl1 Ru S2 C9 3.53(12) . . . . ? O4 Ru S2 C10 -167.6(11) . . . . ? N1 Ru S2 C10 -158.77(13) . . . . ? S3 Ru S2 C10 -67.03(13) . . . . ? S1 Ru S2 C10 30.43(12) . . . . ? Cl1 Ru S2 C10 116.58(13) . . . . ? O4 Ru S3 O3 -136.02(12) . . . . ? N1 Ru S3 O3 145.41(12) . . . . ? S2 Ru S3 O3 46.85(11) . . . . ? S1 Ru S3 O3 -46.37(11) . . . . ? Cl1 Ru S3 O3 -179(54) . . . . ? O4 Ru S3 C12 -11.13(13) . . . . ? N1 Ru S3 C12 -89.69(13) . . . . ? S2 Ru S3 C12 171.74(12) . . . . ? S1 Ru S3 C12 78.53(12) . . . . ? Cl1 Ru S3 C12 -54.1(3) . . . . ? O4 Ru S3 C11 98.83(13) . . . . ? N1 Ru S3 C11 20.26(14) . . . . ? S2 Ru S3 C11 -78.30(13) . . . . ? S1 Ru S3 C11 -171.52(12) . . . . ? Cl1 Ru S3 C11 55.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 29.63 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.326 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.067