Syntheses and Single Crystal X-Ray Diffraction Studies of Acyclic and Macrocyclic Aza-dithiolate (NS2) Complexes of (Arene)ruthenium(II). Base-Promoted Formation of Tethered Arene and Thiolate-alkylation Derivatives. Richard Y. C. Shin, Geok Kheng Tan, Lip Lin Koh and Lai Yoong Goh* Department of Chemistry, National University of Singapore, Kent Ridge, Singapore 119260 E-mail: chmgohly@nus.edu.sg. Fax: (+65) 6779 1691 Complex 2 data_1302a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H30 N2 Ru S2' _chemical_formula_weight 439.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.7421(7) _cell_length_b 11.9068(8) _cell_length_c 16.4702(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1910.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5273 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.52 _exptl_crystal_description Hexagonal plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 1.040 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick, 2001)' _exptl_absorpt_correction_T_min 0.665252 _exptl_absorpt_correction_T_max 0.863713 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15629 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 30.05 _reflns_number_total 5402 _reflns_number_gt 5100 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0437P)^2^+0.2517P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 5402 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 0.38732(2) 0.351444(18) 0.831785(13) 0.02361(7) Uani 1 1 d . . . S1 S 0.59114(10) 0.45321(8) 0.86195(7) 0.0409(2) Uani 1 1 d . . . S2 S 0.37812(11) 0.43854(8) 0.70154(5) 0.0423(2) Uani 1 1 d . . . N1 N 0.5316(3) 0.2402(3) 0.77296(18) 0.0331(6) Uani 1 1 d . . . H1 H 0.512(4) 0.182(3) 0.789(2) 0.023(9) Uiso 1 1 d . . . C1 C 0.7056(5) 0.3416(6) 0.8498(5) 0.118(3) Uani 1 1 d . . . H1A H 0.7949 0.3736 0.8350 0.141 Uiso 1 1 calc R . . H1B H 0.7168 0.3058 0.9030 0.141 Uiso 1 1 calc R . . C2 C 0.6761(5) 0.2581(4) 0.7944(4) 0.0714(16) Uani 1 1 d . . . H2A H 0.7124 0.1873 0.8158 0.086 Uiso 1 1 calc R . . H2B H 0.7265 0.2747 0.7443 0.086 Uiso 1 1 calc R . . C3 C 0.5124(5) 0.2383(3) 0.6837(2) 0.0492(10) Uani 1 1 d . . . H3A H 0.4278 0.1974 0.6708 0.059 Uiso 1 1 calc R . . H3B H 0.5892 0.1982 0.6586 0.059 Uiso 1 1 calc R . . C4 C 0.5041(4) 0.3538(3) 0.6493(2) 0.0469(9) Uani 1 1 d . . . H4A H 0.4799 0.3491 0.5916 0.056 Uiso 1 1 calc R . . H4B H 0.5942 0.3899 0.6535 0.056 Uiso 1 1 calc R . . C5 C 0.3281(4) 0.2272(3) 0.9261(2) 0.0320(7) Uani 1 1 d . . . C6 C 0.2370(4) 0.2146(3) 0.8575(2) 0.0320(7) Uani 1 1 d . . . C7 C 0.1644(3) 0.3071(3) 0.8272(2) 0.0339(7) Uani 1 1 d . . . C8 C 0.1839(3) 0.4167(3) 0.8637(2) 0.0328(7) Uani 1 1 d . . . C9 C 0.2699(3) 0.4284(3) 0.93162(19) 0.0302(7) Uani 1 1 d . . . C10 C 0.3415(4) 0.3331(3) 0.96397(19) 0.0315(6) Uani 1 1 d . . . C11 C 0.4042(5) 0.1252(3) 0.9567(3) 0.0523(11) Uani 1 1 d . . . H11A H 0.4769 0.1487 0.9932 0.079 Uiso 1 1 calc R . . H11B H 0.4437 0.0850 0.9111 0.079 Uiso 1 1 calc R . . H11C H 0.3411 0.0764 0.9854 0.079 Uiso 1 1 calc R . . C12 C 0.2217(5) 0.0997(3) 0.8197(3) 0.0522(11) Uani 1 1 d . . . H12A H 0.1655 0.1052 0.7713 0.078 Uiso 1 1 calc R . . H12B H 0.1782 0.0494 0.8582 0.078 Uiso 1 1 calc R . . H12C H 0.3115 0.0707 0.8054 0.078 Uiso 1 1 calc R . . C13 C 0.0709(4) 0.2955(4) 0.7553(2) 0.0517(11) Uani 1 1 d . . . H13A H 0.1138 0.3293 0.7081 0.078 Uiso 1 1 calc R . . H13B H -0.0153 0.3333 0.7665 0.078 Uiso 1 1 calc R . . H13C H 0.0537 0.2166 0.7449 0.078 Uiso 1 1 calc R . . C14 C 0.1061(4) 0.5154(3) 0.8279(2) 0.0489(9) Uani 1 1 d . . . H14A H 0.0119 0.5141 0.8470 0.073 Uiso 1 1 calc R . . H14B H 0.1072 0.5102 0.7691 0.073 Uiso 1 1 calc R . . H14C H 0.1495 0.5850 0.8446 0.073 Uiso 1 1 calc R . . C15 C 0.2885(5) 0.5410(3) 0.9740(3) 0.0475(10) Uani 1 1 d . . . H15A H 0.2508 0.6002 0.9403 0.071 Uiso 1 1 calc R . . H15B H 0.3855 0.5547 0.9829 0.071 Uiso 1 1 calc R . . H15C H 0.2410 0.5398 1.0257 0.071 Uiso 1 1 calc R . . C16 C 0.4337(5) 0.3490(4) 1.0368(2) 0.0497(9) Uani 1 1 d . . . H16A H 0.4730 0.2772 1.0523 0.075 Uiso 1 1 calc R . . H16B H 0.3806 0.3789 1.0817 0.075 Uiso 1 1 calc R . . H16C H 0.5069 0.4009 1.0232 0.075 Uiso 1 1 calc R . . N1S N 0.8771(5) 0.3242(4) 0.5673(3) 0.0795(13) Uani 1 1 d . . . C1S C 0.7028(5) 0.3221(4) 0.4512(3) 0.0611(12) Uani 1 1 d . . . H1S1 H 0.7088 0.2507 0.4231 0.092 Uiso 1 1 calc R . . H1S2 H 0.7226 0.3826 0.4135 0.092 Uiso 1 1 calc R . . H1S3 H 0.6110 0.3316 0.4729 0.092 Uiso 1 1 calc R . . C2S C 0.8013(5) 0.3243(3) 0.5170(3) 0.0498(10) 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 0.02232(10) 0.02295(10) 0.02555(11) -0.00037(9) 0.00342(9) 0.00077(9) S1 0.0323(5) 0.0356(4) 0.0548(5) -0.0095(4) 0.0055(4) -0.0092(4) S2 0.0441(5) 0.0502(5) 0.0325(4) 0.0110(4) 0.0077(4) 0.0090(5) N1 0.0319(15) 0.0267(15) 0.0407(16) -0.0030(12) 0.0066(12) 0.0006(12) C1 0.035(3) 0.110(5) 0.208(8) -0.082(6) -0.042(4) 0.019(3) C2 0.031(2) 0.062(3) 0.121(4) -0.039(3) -0.010(3) 0.017(2) C3 0.068(3) 0.041(2) 0.040(2) -0.0107(16) 0.0190(19) -0.0028(18) C4 0.053(2) 0.052(2) 0.0353(17) -0.0005(17) 0.0130(16) 0.004(2) C5 0.0354(17) 0.0275(14) 0.0330(16) 0.0068(12) 0.0067(14) 0.0005(13) C6 0.0311(17) 0.0337(16) 0.0311(16) -0.0037(13) 0.0088(13) -0.0064(13) C7 0.0232(14) 0.0465(17) 0.0321(16) -0.0015(15) 0.0077(14) -0.0057(13) C8 0.0237(16) 0.0402(18) 0.0346(16) 0.0035(14) 0.0100(13) 0.0043(13) C9 0.0331(17) 0.0301(15) 0.0274(15) 0.0007(12) 0.0090(13) -0.0017(13) C10 0.0332(16) 0.0349(16) 0.0264(14) 0.0020(12) 0.0051(12) -0.0009(13) C11 0.066(3) 0.0368(19) 0.055(2) 0.0140(16) 0.010(2) 0.0114(19) C12 0.056(3) 0.0420(19) 0.059(3) -0.0169(19) 0.012(2) -0.0136(18) C13 0.032(2) 0.079(3) 0.043(2) -0.012(2) -0.0025(17) -0.006(2) C14 0.041(2) 0.053(2) 0.052(2) 0.0113(18) 0.007(2) 0.0167(17) C15 0.061(3) 0.0345(18) 0.047(2) -0.0109(16) 0.0142(19) -0.0062(18) C16 0.057(2) 0.058(2) 0.0342(17) -0.0001(19) -0.0087(16) -0.009(2) N1S 0.076(3) 0.070(3) 0.092(3) 0.005(2) -0.014(3) -0.005(3) C1S 0.056(3) 0.064(3) 0.063(3) 0.011(2) 0.005(2) -0.012(2) C2S 0.051(3) 0.042(2) 0.056(3) 0.0052(18) 0.010(2) -0.0042(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 Ru1 N1 2.161(3) . ? Ru1 C8 2.193(3) . ? Ru1 C9 2.203(3) . ? Ru1 C5 2.222(3) . ? Ru1 C6 2.231(3) . ? Ru1 C10 2.233(3) . ? Ru1 C7 2.236(3) . ? Ru1 S1 2.3786(9) . ? Ru1 S2 2.3844(9) . ? S1 C1 1.746(6) . ? S2 C4 1.807(4) . ? N1 C2 1.467(5) . ? N1 C3 1.482(5) . ? C1 C2 1.380(7) . ? C3 C4 1.490(6) . ? C5 C10 1.413(4) . ? C5 C6 1.445(5) . ? C5 C11 1.509(5) . ? C6 C7 1.401(5) . ? C6 C12 1.510(5) . ? C7 C8 1.449(5) . ? C7 C13 1.501(5) . ? C8 C9 1.404(5) . ? C8 C14 1.518(5) . ? C9 C10 1.435(4) . ? C9 C15 1.521(5) . ? C10 C16 1.511(5) . ? N1S C2S 1.110(6) . ? C1S C2S 1.448(7) . ? 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 C8 155.89(13) . . ? N1 Ru1 C9 158.06(12) . . ? C8 Ru1 C9 37.26(13) . . ? N1 Ru1 C5 94.25(12) . . ? C8 Ru1 C5 80.42(13) . . ? C9 Ru1 C5 67.69(12) . . ? N1 Ru1 C6 93.69(12) . . ? C8 Ru1 C6 67.67(13) . . ? C9 Ru1 C6 79.72(12) . . ? C5 Ru1 C6 37.88(13) . . ? N1 Ru1 C10 120.48(12) . . ? C8 Ru1 C10 67.66(13) . . ? C9 Ru1 C10 37.74(12) . . ? C5 Ru1 C10 36.97(12) . . ? C6 Ru1 C10 67.19(12) . . ? N1 Ru1 C7 118.17(12) . . ? C8 Ru1 C7 38.18(13) . . ? C9 Ru1 C7 67.61(13) . . ? C5 Ru1 C7 67.31(13) . . ? C6 Ru1 C7 36.54(13) . . ? C10 Ru1 C7 79.36(13) . . ? N1 Ru1 S1 82.11(9) . . ? C8 Ru1 S1 121.60(10) . . ? C9 Ru1 S1 93.76(9) . . ? C5 Ru1 S1 114.19(10) . . ? C6 Ru1 S1 151.67(10) . . ? C10 Ru1 S1 90.76(9) . . ? C7 Ru1 S1 159.72(9) . . ? N1 Ru1 S2 83.55(9) . . ? C8 Ru1 S2 91.60(9) . . ? C9 Ru1 S2 118.10(9) . . ? C5 Ru1 S2 155.38(10) . . ? C6 Ru1 S2 117.62(9) . . ? C10 Ru1 S2 155.80(9) . . ? C7 Ru1 S2 92.06(10) . . ? S1 Ru1 S2 89.87(4) . . ? C1 S1 Ru1 96.99(19) . . ? C4 S2 Ru1 99.20(12) . . ? C2 N1 C3 111.3(4) . . ? C2 N1 Ru1 115.3(2) . . ? C3 N1 Ru1 111.8(2) . . ? C2 C1 S1 119.4(4) . . ? C1 C2 N1 117.6(4) . . ? N1 C3 C4 111.7(3) . . ? C3 C4 S2 111.8(3) . . ? C10 C5 C6 119.6(3) . . ? C10 C5 C11 121.7(3) . . ? C6 C5 C11 118.7(3) . . ? C10 C5 Ru1 71.96(17) . . ? C6 C5 Ru1 71.43(18) . . ? C11 C5 Ru1 129.9(3) . . ? C7 C6 C5 120.5(3) . . ? C7 C6 C12 121.1(3) . . ? C5 C6 C12 118.5(3) . . ? C7 C6 Ru1 71.91(19) . . ? C5 C6 Ru1 70.70(18) . . ? C12 C6 Ru1 130.4(3) . . ? C6 C7 C8 119.6(3) . . ? C6 C7 C13 121.0(3) . . ? C8 C7 C13 119.3(3) . . ? C6 C7 Ru1 71.5(2) . . ? C8 C7 Ru1 69.30(18) . . ? C13 C7 Ru1 129.6(3) . . ? C9 C8 C7 119.9(3) . . ? C9 C8 C14 122.0(3) . . ? C7 C8 C14 118.1(3) . . ? C9 C8 Ru1 71.76(19) . . ? C7 C8 Ru1 72.52(19) . . ? C14 C8 Ru1 129.2(2) . . ? C8 C9 C10 120.4(3) . . ? C8 C9 C15 121.6(3) . . ? C10 C9 C15 118.0(3) . . ? C8 C9 Ru1 70.99(19) . . ? C10 C9 Ru1 72.27(18) . . ? C15 C9 Ru1 130.3(2) . . ? C5 C10 C9 119.9(3) . . ? C5 C10 C16 121.1(3) . . ? C9 C10 C16 119.0(3) . . ? C5 C10 Ru1 71.07(17) . . ? C9 C10 Ru1 69.99(17) . . ? C16 C10 Ru1 130.0(3) . . ? N1S C2S C1S 178.9(5) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.894 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.095 #===END Complex 3 data_2020a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H34 F12 N2 O2 P2 Ru S2' _chemical_formula_weight 777.61 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 17.7539(11) _cell_length_b 11.8517(8) _cell_length_c 13.7702(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2897.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6873 _cell_measurement_theta_min 2.267 _cell_measurement_theta_max 27.628 _exptl_crystal_description Rectangular Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.895 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick, 2001)' _exptl_absorpt_correction_T_min 0.8849 _exptl_absorpt_correction_T_max 0.9158 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19349 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5086 _reflns_number_gt 4670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0837P)^2^+3.6823P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(7) _refine_ls_number_reflns 5086 _refine_ls_number_parameters 354 _refine_ls_number_restraints 653 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1330 _refine_ls_wR_factor_gt 0.1294 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.260 _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 Ru1 Ru 0.19161(2) 0.12815(3) 0.84618(6) 0.02855(15) Uani 1 1 d . . . S1 S 0.18584(10) 0.04822(16) 0.69200(15) 0.0412(4) Uani 1 1 d . . . S2 S 0.07131(9) 0.19679(16) 0.81834(15) 0.0428(4) Uani 1 1 d . . . N1 N 0.2256(4) 0.2756(5) 0.7661(5) 0.0391(13) Uani 1 1 d . . . H1 H 0.249(4) 0.307(6) 0.803(6) 0.024(18) Uiso 1 1 d . . . C1 C 0.2218(5) 0.1611(8) 0.6143(7) 0.054(2) Uani 1 1 d . . . H1A H 0.2536 0.1293 0.5629 0.065 Uiso 1 1 calc R . . H1B H 0.1798 0.2014 0.5838 0.065 Uiso 1 1 calc R . . C2 C 0.2680(5) 0.2424(8) 0.6775(6) 0.0515(19) Uani 1 1 d . . . H2A H 0.3153 0.2060 0.6964 0.062 Uiso 1 1 calc R . . H2B H 0.2803 0.3100 0.6397 0.062 Uiso 1 1 calc R . . C3 C 0.1646(6) 0.3578(7) 0.7401(9) 0.057(2) Uani 1 1 d . . . H3A H 0.1504 0.3470 0.6720 0.069 Uiso 1 1 calc R . . H3B H 0.1838 0.4349 0.7473 0.069 Uiso 1 1 calc R . . C4 C 0.0960(5) 0.3434(7) 0.8032(8) 0.056(2) Uani 1 1 d . . . H4A H 0.0535 0.3836 0.7738 0.068 Uiso 1 1 calc R . . H4B H 0.1057 0.3769 0.8670 0.068 Uiso 1 1 calc R . . C5 C 0.0463(5) 0.1553(8) 0.6933(7) 0.0499(18) Uani 1 1 d . . . H5A H -0.0083 0.1438 0.6889 0.060 Uiso 1 1 calc R . . H5B H 0.0600 0.2162 0.6484 0.060 Uiso 1 1 calc R . . C6 C 0.0856(5) 0.0502(7) 0.6644(7) 0.0488(19) Uani 1 1 d . . . H6A H 0.0791 0.0392 0.5944 0.059 Uiso 1 1 calc R . . H6B H 0.0616 -0.0136 0.6974 0.059 Uiso 1 1 calc R . . C7 C 0.2978(4) 0.1218(6) 0.9357(7) 0.0420(18) Uani 1 1 d . . . C8 C 0.2398(5) 0.1819(7) 0.9895(6) 0.0433(17) Uani 1 1 d . . . C9 C 0.1705(5) 0.1319(7) 1.0059(7) 0.0467(19) Uani 1 1 d . . . C10 C 0.1562(4) 0.0187(7) 0.9698(6) 0.0445(17) Uani 1 1 d . . . C11 C 0.2112(4) -0.0383(6) 0.9165(7) 0.0435(17) Uani 1 1 d . . . C12 C 0.2842(4) 0.0131(6) 0.9005(6) 0.0397(16) Uani 1 1 d . . . C13 C 0.3739(5) 0.1762(9) 0.9169(9) 0.063(3) Uani 1 1 d . . . H13A H 0.4117 0.1407 0.9576 0.094 Uiso 1 1 calc R . . H13B H 0.3712 0.2560 0.9319 0.094 Uiso 1 1 calc R . . H13C H 0.3874 0.1664 0.8491 0.094 Uiso 1 1 calc R . . C14 C 0.2558(7) 0.3014(8) 1.0272(9) 0.070(3) Uani 1 1 d . . . H14A H 0.2117 0.3299 1.0608 0.105 Uiso 1 1 calc R . . H14B H 0.2676 0.3505 0.9729 0.105 Uiso 1 1 calc R . . H14C H 0.2982 0.2993 1.0716 0.105 Uiso 1 1 calc R . . C15 C 0.1082(7) 0.1934(10) 1.0606(8) 0.076(3) Uani 1 1 d . . . H15A H 0.1026 0.2690 1.0346 0.114 Uiso 1 1 calc R . . H15B H 0.1211 0.1977 1.1289 0.114 Uiso 1 1 calc R . . H15C H 0.0612 0.1526 1.0530 0.114 Uiso 1 1 calc R . . C16 C 0.0799(5) -0.0352(10) 0.9907(11) 0.077(4) Uani 1 1 d . . . H16A H 0.0826 -0.0772 1.0511 0.116 Uiso 1 1 calc R . . H16B H 0.0667 -0.0859 0.9381 0.116 Uiso 1 1 calc R . . H16C H 0.0419 0.0233 0.9963 0.116 Uiso 1 1 calc R . . C17 C 0.1978(6) -0.1557(7) 0.8784(10) 0.071(3) Uani 1 1 d . . . H17A H 0.1441 -0.1684 0.8717 0.107 Uiso 1 1 calc R . . H17B H 0.2187 -0.2103 0.9234 0.107 Uiso 1 1 calc R . . H17C H 0.2219 -0.1639 0.8156 0.107 Uiso 1 1 calc R . . C18 C 0.3440(4) -0.0523(7) 0.8465(10) 0.061(2) Uani 1 1 d . . . H18A H 0.3815 -0.0004 0.8213 0.092 Uiso 1 1 calc R . . H18B H 0.3210 -0.0931 0.7931 0.092 Uiso 1 1 calc R . . H18C H 0.3679 -0.1053 0.8904 0.092 Uiso 1 1 calc R . . N1S N 0.0812(5) 0.6965(7) 0.7007(8) 0.065(2) Uani 1 1 d . . . O1S O 0.1321(6) 0.6343(9) 0.6967(14) 0.131(6) Uani 1 1 d . . . O2S O 0.0751(5) 0.7810(7) 0.6534(8) 0.092(3) Uani 1 1 d . . . C1S C 0.0192(9) 0.6740(10) 0.7684(11) 0.092(4) Uani 1 1 d . . . H1SA H 0.0290 0.6043 0.8032 0.138 Uiso 1 1 calc R . . H1SB H -0.0276 0.6671 0.7325 0.138 Uiso 1 1 calc R . . H1SC H 0.0151 0.7357 0.8144 0.138 Uiso 1 1 calc R . . P1 P 0.13722(12) 0.04552(18) 0.3370(2) 0.0588(6) Uani 1 1 d D . . F1 F 0.2166(4) 0.0204(8) 0.3835(7) 0.123(3) Uani 1 1 d D . . F2 F 0.1445(6) -0.0603(9) 0.2741(10) 0.212(9) Uani 1 1 d D . . F3 F 0.0578(3) 0.0664(6) 0.2896(6) 0.090(2) Uani 1 1 d D . . F4 F 0.1276(7) 0.1482(8) 0.4056(11) 0.216(10) Uani 1 1 d D . . F5 F 0.0982(5) -0.0278(9) 0.4192(8) 0.146(5) Uani 1 1 d D . . F6 F 0.1743(6) 0.1230(13) 0.2625(10) 0.235(13) Uani 1 1 d D . . P2 P -0.04796(13) 0.43219(17) 0.55651(18) 0.0486(5) Uani 1 1 d D . . F7 F -0.0795(7) 0.3154(9) 0.5402(11) 0.100(2) Uiso 0.50 1 d PD A 1 F8 F 0.0354(6) 0.3935(11) 0.5533(12) 0.100(2) Uiso 0.50 1 d PD A 1 F9 F -0.0205(8) 0.5593(8) 0.5788(11) 0.100(2) Uiso 0.50 1 d PD A 1 F10 F -0.1302(6) 0.4812(11) 0.5697(12) 0.100(2) Uiso 0.50 1 d PD A 1 F11 F -0.0468(8) 0.4085(12) 0.6703(8) 0.100(2) Uiso 0.50 1 d PD A 1 F12 F -0.0452(8) 0.4642(12) 0.4488(9) 0.100(2) Uiso 0.50 1 d PD A 1 F7A F -0.1117(8) 0.3735(13) 0.5002(13) 0.111(2) Uiso 0.50 1 d PD A 2 F8A F 0.0097(9) 0.3389(11) 0.5141(12) 0.111(2) Uiso 0.50 1 d PD A 2 F9A F 0.0211(7) 0.4794(12) 0.6135(11) 0.111(2) Uiso 0.50 1 d PD A 2 F10A F -0.1051(8) 0.5127(12) 0.6039(14) 0.111(2) Uiso 0.50 1 d PD A 2 F11A F -0.0617(9) 0.3499(12) 0.6468(11) 0.111(2) Uiso 0.50 1 d PD A 2 F12A F -0.0262(10) 0.5065(12) 0.4673(11) 0.111(2) Uiso 0.50 1 d PD 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 0.0282(2) 0.0294(2) 0.0280(2) 0.0006(2) -0.0010(2) 0.00430(15) S1 0.0475(10) 0.0394(9) 0.0365(10) -0.0075(8) -0.0023(8) 0.0072(7) S2 0.0333(7) 0.0541(9) 0.0409(10) 0.0006(8) -0.0026(7) 0.0123(7) N1 0.044(3) 0.035(3) 0.038(3) 0.004(3) -0.007(3) -0.005(2) C1 0.059(5) 0.069(5) 0.035(4) -0.002(4) 0.007(4) 0.001(4) C2 0.053(4) 0.065(5) 0.037(4) 0.010(4) 0.002(3) -0.014(4) C3 0.071(6) 0.038(4) 0.063(6) 0.013(4) -0.016(5) 0.001(4) C4 0.064(5) 0.046(4) 0.059(5) 0.000(4) -0.009(4) 0.029(4) C5 0.042(4) 0.064(4) 0.043(5) -0.004(4) -0.017(4) 0.002(3) C6 0.055(4) 0.045(4) 0.047(5) 0.003(4) -0.013(4) -0.009(3) C7 0.036(3) 0.044(4) 0.046(5) 0.002(3) -0.009(3) 0.004(3) C8 0.056(4) 0.045(4) 0.029(4) -0.002(3) -0.007(3) 0.012(3) C9 0.044(4) 0.060(5) 0.036(4) 0.007(4) -0.003(3) 0.016(3) C10 0.040(4) 0.051(4) 0.041(4) 0.018(4) 0.002(3) 0.003(3) C11 0.041(3) 0.036(3) 0.053(5) 0.010(3) -0.004(3) 0.004(3) C12 0.033(3) 0.045(4) 0.042(4) 0.005(3) -0.003(3) 0.011(3) C13 0.040(4) 0.070(6) 0.079(7) -0.002(6) -0.016(4) -0.007(4) C14 0.094(7) 0.056(5) 0.059(6) -0.015(5) -0.024(6) 0.012(5) C15 0.092(7) 0.096(8) 0.040(5) 0.004(6) 0.022(5) 0.031(6) C16 0.046(5) 0.092(7) 0.093(9) 0.039(7) 0.016(5) -0.007(5) C17 0.094(7) 0.033(4) 0.087(9) 0.011(5) -0.017(6) -0.011(4) C18 0.048(4) 0.057(4) 0.078(6) -0.013(6) 0.012(5) 0.023(3) N1S 0.071(5) 0.046(4) 0.079(6) -0.009(4) 0.000(5) -0.003(3) O1S 0.077(6) 0.109(7) 0.208(18) 0.014(8) -0.011(8) 0.031(5) O2S 0.106(6) 0.064(4) 0.105(8) 0.022(5) 0.032(6) 0.001(4) C1S 0.143(12) 0.069(7) 0.064(8) 0.011(6) 0.024(8) -0.022(7) P1 0.0548(10) 0.0571(10) 0.0646(16) 0.0102(14) -0.0135(13) 0.0036(8) F1 0.073(4) 0.175(9) 0.120(8) 0.036(7) -0.044(5) 0.013(5) F2 0.128(8) 0.198(11) 0.31(2) -0.168(13) -0.086(10) 0.091(8) F3 0.071(4) 0.097(4) 0.101(6) 0.009(4) -0.025(4) 0.016(3) F4 0.217(15) 0.112(7) 0.32(2) -0.090(11) -0.146(17) 0.038(8) F5 0.098(6) 0.169(9) 0.169(12) 0.079(9) 0.026(7) 0.017(6) F6 0.126(9) 0.38(3) 0.194(17) 0.200(19) -0.061(10) -0.110(12) P2 0.0556(11) 0.0451(10) 0.0451(12) 0.0053(9) -0.0035(10) 0.0037(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.153(6) . ? Ru1 C11 2.225(7) . ? Ru1 C9 2.231(10) . ? Ru1 C10 2.231(8) . ? Ru1 C8 2.243(8) . ? Ru1 C7 2.253(8) . ? Ru1 C12 2.262(7) . ? Ru1 S2 2.3175(16) . ? Ru1 S1 2.327(2) . ? S1 C6 1.819(8) . ? S1 C1 1.828(10) . ? S2 C4 1.804(9) . ? S2 C5 1.845(9) . ? N1 C2 1.487(12) . ? N1 C3 1.501(11) . ? C1 C2 1.536(13) . ? C3 C4 1.506(15) . ? C5 C6 1.483(12) . ? C7 C12 1.398(11) . ? C7 C8 1.454(12) . ? C7 C13 1.519(11) . ? C8 C9 1.384(13) . ? C8 C14 1.535(12) . ? C9 C10 1.453(13) . ? C9 C15 1.525(13) . ? C10 C11 1.396(12) . ? C10 C16 1.524(11) . ? C11 C12 1.448(11) . ? C11 C17 1.506(12) . ? C12 C18 1.510(10) . ? N1S O1S 1.167(12) . ? N1S O2S 1.199(12) . ? N1S C1S 1.468(16) . ? P1 F6 1.526(8) . ? P1 F2 1.530(8) . ? P1 F4 1.550(9) . ? P1 F3 1.573(6) . ? P1 F1 1.576(6) . ? P1 F5 1.587(8) . ? P2 F7 1.510(10) . ? P2 F12 1.532(12) . ? P2 F10A 1.538(13) . ? P2 F7A 1.538(13) . ? P2 F8 1.550(10) . ? P2 F9A 1.560(12) . ? P2 F12A 1.561(13) . ? P2 F10 1.582(9) . ? P2 F11 1.592(10) . ? P2 F11A 1.599(13) . ? P2 F9 1.613(9) . ? P2 F8A 1.616(12) . ? 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 C11 154.0(3) . . ? N1 Ru1 C9 122.4(3) . . ? C11 Ru1 C9 67.4(3) . . ? N1 Ru1 C10 160.4(3) . . ? C11 Ru1 C10 36.5(3) . . ? C9 Ru1 C10 38.0(3) . . ? N1 Ru1 C8 96.5(3) . . ? C11 Ru1 C8 79.0(3) . . ? C9 Ru1 C8 36.0(3) . . ? C10 Ru1 C8 66.5(3) . . ? N1 Ru1 C7 94.2(3) . . ? C11 Ru1 C7 66.5(3) . . ? C9 Ru1 C7 66.5(3) . . ? C10 Ru1 C7 78.4(3) . . ? C8 Ru1 C7 37.7(3) . . ? N1 Ru1 C12 117.1(3) . . ? C11 Ru1 C12 37.6(3) . . ? C9 Ru1 C12 78.9(3) . . ? C10 Ru1 C12 66.5(3) . . ? C8 Ru1 C12 66.6(3) . . ? C7 Ru1 C12 36.1(3) . . ? N1 Ru1 S2 83.62(18) . . ? C11 Ru1 S2 121.8(2) . . ? C9 Ru1 S2 90.1(2) . . ? C10 Ru1 S2 94.0(2) . . ? C8 Ru1 S2 113.4(2) . . ? C7 Ru1 S2 150.8(2) . . ? C12 Ru1 S2 159.3(2) . . ? N1 Ru1 S1 82.9(2) . . ? C11 Ru1 S1 92.5(2) . . ? C9 Ru1 S1 154.2(2) . . ? C10 Ru1 S1 116.6(3) . . ? C8 Ru1 S1 159.2(2) . . ? C7 Ru1 S1 121.5(2) . . ? C12 Ru1 S1 95.1(2) . . ? S2 Ru1 S1 87.21(7) . . ? C6 S1 C1 102.1(4) . . ? C6 S1 Ru1 103.2(3) . . ? C1 S1 Ru1 102.8(3) . . ? C4 S2 C5 102.0(5) . . ? C4 S2 Ru1 97.7(3) . . ? C5 S2 Ru1 106.4(3) . . ? C2 N1 C3 110.0(8) . . ? C2 N1 Ru1 110.3(5) . . ? C3 N1 Ru1 116.5(5) . . ? C2 C1 S1 108.3(6) . . ? N1 C2 C1 111.1(7) . . ? N1 C3 C4 111.9(7) . . ? C3 C4 S2 111.9(6) . . ? C6 C5 S2 111.1(6) . . ? C5 C6 S1 114.6(6) . . ? C12 C7 C8 120.4(7) . . ? C12 C7 C13 119.1(8) . . ? C8 C7 C13 120.6(8) . . ? C12 C7 Ru1 72.3(4) . . ? C8 C7 Ru1 70.8(4) . . ? C13 C7 Ru1 129.5(7) . . ? C9 C8 C7 120.2(7) . . ? C9 C8 C14 120.3(8) . . ? C7 C8 C14 119.5(8) . . ? C9 C8 Ru1 71.5(5) . . ? C7 C8 Ru1 71.5(5) . . ? C14 C8 Ru1 129.1(6) . . ? C8 C9 C10 119.7(8) . . ? C8 C9 C15 121.4(9) . . ? C10 C9 C15 118.9(9) . . ? C8 C9 Ru1 72.5(5) . . ? C10 C9 Ru1 71.0(5) . . ? C15 C9 Ru1 128.2(6) . . ? C11 C10 C9 120.2(7) . . ? C11 C10 C16 121.2(9) . . ? C9 C10 C16 118.6(8) . . ? C11 C10 Ru1 71.5(4) . . ? C9 C10 Ru1 71.0(5) . . ? C16 C10 Ru1 129.7(7) . . ? C10 C11 C12 120.2(7) . . ? C10 C11 C17 121.3(8) . . ? C12 C11 C17 118.5(8) . . ? C10 C11 Ru1 72.0(4) . . ? C12 C11 Ru1 72.6(4) . . ? C17 C11 Ru1 130.0(7) . . ? C7 C12 C11 119.3(7) . . ? C7 C12 C18 121.5(7) . . ? C11 C12 C18 119.2(7) . . ? C7 C12 Ru1 71.6(4) . . ? C11 C12 Ru1 69.8(4) . . ? C18 C12 Ru1 131.1(7) . . ? O1S N1S O2S 124.9(13) . . ? O1S N1S C1S 119.7(12) . . ? O2S N1S C1S 115.4(9) . . ? F6 P1 F2 94.4(8) . . ? F6 P1 F4 89.1(6) . . ? F2 P1 F4 176.5(8) . . ? F6 P1 F3 90.8(5) . . ? F2 P1 F3 88.3(4) . . ? F4 P1 F3 91.7(5) . . ? F6 P1 F1 90.1(5) . . ? F2 P1 F1 90.0(5) . . ? F4 P1 F1 89.9(5) . . ? F3 P1 F1 178.1(5) . . ? F6 P1 F5 176.1(8) . . ? F2 P1 F5 89.5(6) . . ? F4 P1 F5 87.0(7) . . ? F3 P1 F5 89.5(5) . . ? F1 P1 F5 89.8(5) . . ? F7 P2 F12 95.5(7) . . ? F7 P2 F10A 112.8(8) . . ? F12 P2 F10A 106.2(9) . . ? F7 P2 F7A 40.3(7) . . ? F12 P2 F7A 69.4(9) . . ? F10A P2 F7A 90.5(7) . . ? F7 P2 F8 94.5(6) . . ? F12 P2 F8 90.9(7) . . ? F10A P2 F8 145.6(8) . . ? F7A P2 F8 123.7(8) . . ? F7 P2 F9A 134.0(8) . . ? F12 P2 F9A 111.9(8) . . ? F10A P2 F9A 94.7(7) . . ? F7A P2 F9A 173.9(8) . . ? F8 P2 F9A 50.9(7) . . ? F7 P2 F12A 119.5(8) . . ? F12 P2 F12A 24.5(7) . . ? F10A P2 F12A 98.5(9) . . ? F7A P2 F12A 92.4(8) . . ? F8 P2 F12A 84.7(9) . . ? F9A P2 F12A 89.9(7) . . ? F7 P2 F10 90.6(6) . . ? F12 P2 F10 92.8(7) . . ? F10A P2 F10 27.7(7) . . ? F7A P2 F10 62.9(8) . . ? F8 P2 F10 173.3(8) . . ? F9A P2 F10 122.5(7) . . ? F12A P2 F10 96.4(9) . . ? F7 P2 F11 89.4(7) . . ? F12 P2 F11 175.1(8) . . ? F10A P2 F11 72.6(9) . . ? F7A P2 F11 115.2(8) . . ? F8 P2 F11 87.9(7) . . ? F9A P2 F11 63.7(7) . . ? F12A P2 F11 150.6(8) . . ? F10 P2 F11 88.0(6) . . ? F7 P2 F11A 59.9(8) . . ? F12 P2 F11A 155.3(8) . . ? F10A P2 F11A 87.0(8) . . ? F7A P2 F11A 90.2(7) . . ? F8 P2 F11A 89.3(8) . . ? F9A P2 F11A 87.0(7) . . ? F12A P2 F11A 173.9(8) . . ? F10 P2 F11A 89.6(8) . . ? F11 P2 F11A 29.5(7) . . ? F7 P2 F9 175.3(7) . . ? F12 P2 F9 86.8(6) . . ? F10A P2 F9 62.6(7) . . ? F7A P2 F9 137.8(8) . . ? F8 P2 F9 89.6(6) . . ? F9A P2 F9 48.0(7) . . ? F12A P2 F9 63.1(8) . . ? F10 P2 F9 85.1(6) . . ? F11 P2 F9 88.4(7) . . ? F11A P2 F9 117.9(8) . . ? F7 P2 F8A 63.5(7) . . ? F12 P2 F8A 78.4(9) . . ? F10A P2 F8A 174.7(9) . . ? F7A P2 F8A 88.5(7) . . ? F8 P2 F8A 35.2(7) . . ? F9A P2 F8A 85.9(7) . . ? F12A P2 F8A 86.8(8) . . ? F10 P2 F8A 151.3(8) . . ? F11 P2 F8A 103.1(8) . . ? F11A P2 F8A 87.7(7) . . ? F9 P2 F8A 121.1(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.838 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.107 #===END Complex 5 data_2053 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H41 F12 N3 O4 P2 Ru S2' _chemical_formula_weight 866.71 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1429(5) _cell_length_b 10.6403(5) _cell_length_c 16.5359(8) _cell_angle_alpha 108.2100(10) _cell_angle_beta 98.1320(10) _cell_angle_gamma 93.9630(10) _cell_volume 1665.96(14) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8477 _cell_measurement_theta_min 2.614 _cell_measurement_theta_max 29.983 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.6924 _exptl_absorpt_correction_T_max 0.8324 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21453 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7632 _reflns_number_gt 7206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0548P)^2^+0.9253P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7632 _refine_ls_number_parameters 604 _refine_ls_number_restraints 694 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0897 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.193 _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 0.761148(16) 0.706030(16) 0.265541(11) 0.02743(7) Uani 1 1 d . . . S1 S 0.93264(6) 0.88467(6) 0.31598(4) 0.03586(14) Uani 1 1 d . . . S2 S 0.66863(7) 0.73846(7) 0.13726(4) 0.03860(14) Uani 1 1 d . . . N1 N 0.9053(2) 0.6102(2) 0.19018(14) 0.0350(4) Uani 1 1 d . . . H1 H 0.903(3) 0.531(4) 0.188(2) 0.046(9) Uiso 1 1 d . . . C1 C 1.0590(3) 0.8192(3) 0.2514(2) 0.0476(6) Uani 1 1 d . . . H1A H 1.045(4) 0.846(3) 0.194(2) 0.053(9) Uiso 1 1 d . . . H1B H 1.146(4) 0.856(4) 0.284(3) 0.063(11) Uiso 1 1 d . . . C2 C 1.0453(3) 0.6709(3) 0.2319(2) 0.0449(6) Uani 1 1 d . . . H2A H 1.065(3) 0.646(3) 0.285(2) 0.042(8) Uiso 1 1 d . . . H2B H 1.103(4) 0.634(4) 0.195(3) 0.061(10) Uiso 1 1 d . . . C3 C 0.8799(3) 0.6001(3) 0.09625(18) 0.0466(6) Uani 1 1 d . . . H3A H 0.911(4) 0.522(4) 0.065(2) 0.058(10) Uiso 1 1 d . . . H3B H 0.934(4) 0.685(4) 0.096(2) 0.053(9) Uiso 1 1 d . . . C4 C 0.7339(4) 0.6003(3) 0.06453(18) 0.0489(7) Uani 1 1 d . . . H4A H 0.679(4) 0.521(4) 0.065(2) 0.054(9) Uiso 1 1 d . . . H4B H 0.720(4) 0.607(4) 0.008(3) 0.060(10) Uiso 1 1 d . . . C5 C 0.7492(4) 0.8767(3) 0.11240(19) 0.0450(6) Uani 1 1 d . . . H5A H 0.721(4) 0.856(4) 0.051(2) 0.053(9) Uiso 1 1 d . . . H5B H 0.835(4) 0.875(4) 0.118(2) 0.051(10) Uiso 1 1 d . . . C6 C 0.7121(4) 1.0091(3) 0.1648(2) 0.0518(7) Uani 1 1 d . . . H6A H 0.617(4) 1.015(4) 0.156(3) 0.062(11) Uiso 1 1 d . . . H6B H 0.758(4) 1.078(4) 0.141(3) 0.073(12) Uiso 1 1 d . . . C7 C 0.7544(3) 1.0478(3) 0.2619(2) 0.0471(6) Uani 1 1 d . . . H7A H 0.700(3) 0.993(3) 0.284(2) 0.045(8) Uiso 1 1 d . . . H7B H 0.741(4) 1.135(4) 0.286(2) 0.053(9) Uiso 1 1 d . . . C8 C 0.9005(3) 1.0388(3) 0.2923(2) 0.0486(7) Uani 1 1 d . . . H8A H 0.953(4) 1.046(4) 0.250(2) 0.055(10) Uiso 1 1 d . . . H8B H 0.943(5) 1.110(5) 0.343(3) 0.086(14) Uiso 1 1 d . . . C9 C 0.7778(3) 0.6941(3) 0.40106(17) 0.0417(6) Uani 1 1 d . . . C10 C 0.7684(3) 0.5656(3) 0.34171(18) 0.0394(5) Uani 1 1 d . . . C11 C 0.6566(3) 0.5179(3) 0.27267(18) 0.0413(6) Uani 1 1 d . . . C12 C 0.5587(3) 0.6007(3) 0.2627(2) 0.0448(6) Uani 1 1 d . . . C13 C 0.5728(3) 0.7354(3) 0.3192(2) 0.0455(6) Uani 1 1 d . . . C14 C 0.6809(3) 0.7814(3) 0.38851(18) 0.0434(6) Uani 1 1 d . . . C15 C 0.8913(4) 0.7408(5) 0.4775(2) 0.0713(10) Uani 1 1 d . . . H15A H 0.8834 0.8313 0.5121 0.107 Uiso 1 1 calc R . . H15B H 0.9764 0.7382 0.4570 0.107 Uiso 1 1 calc R . . H15C H 0.8868 0.6828 0.5123 0.107 Uiso 1 1 calc R . . C16 C 0.8721(4) 0.4733(5) 0.3510(3) 0.0627(10) Uani 1 1 d . . . H16A H 0.904(6) 0.417(6) 0.300(4) 0.12(2) Uiso 1 1 d . . . H16B H 0.940(5) 0.525(5) 0.382(3) 0.088(17) Uiso 1 1 d . . . H16C H 0.844(5) 0.417(5) 0.379(3) 0.088(15) Uiso 1 1 d . . . C17 C 0.6420(6) 0.3756(4) 0.2120(3) 0.0726(12) Uani 1 1 d . . . H17A H 0.729(7) 0.346(6) 0.211(4) 0.12(2) Uiso 1 1 d . . . H17B H 0.604(6) 0.317(6) 0.232(4) 0.109(18) Uiso 1 1 d . . . H17C H 0.629(7) 0.373(6) 0.161(5) 0.12(2) Uiso 1 1 d . . . C18 C 0.4365(4) 0.5492(6) 0.1926(4) 0.0830(16) Uani 1 1 d . . . H18A H 0.469(7) 0.462(8) 0.146(5) 0.15(3) Uiso 1 1 d . . . H18B H 0.415(6) 0.611(6) 0.167(4) 0.12(2) Uiso 1 1 d . . . H18C H 0.382(8) 0.516(7) 0.207(5) 0.14(3) Uiso 1 1 d . . . C19 C 0.4683(4) 0.8262(6) 0.3072(4) 0.0799(15) Uani 1 1 d . . . H19A H 0.502(7) 0.926(7) 0.327(5) 0.14(2) Uiso 1 1 d . . . H19B H 0.397(6) 0.821(5) 0.331(4) 0.101(17) Uiso 1 1 d . . . H19C H 0.439(6) 0.812(6) 0.249(4) 0.098(18) Uiso 1 1 d . . . C20 C 0.6958(6) 0.9199(4) 0.4527(3) 0.0762(13) Uani 1 1 d . . . H20A H 0.658(6) 0.979(6) 0.425(4) 0.107(18) Uiso 1 1 d . . . H20B H 0.658(5) 0.917(5) 0.499(3) 0.089(15) Uiso 1 1 d . . . H20C H 0.786(7) 0.955(6) 0.462(4) 0.12(2) Uiso 1 1 d . . . P1 P 0.30462(7) 0.67725(7) 0.47895(5) 0.04424(16) Uani 1 1 d D . . F1 F 0.3896(4) 0.6104(3) 0.4090(3) 0.1246(14) Uani 1 1 d D . . F2 F 0.3577(3) 0.5891(3) 0.5342(2) 0.0973(9) Uani 1 1 d D . . F3 F 0.2172(3) 0.7471(3) 0.54830(17) 0.0915(8) Uani 1 1 d D . . F4 F 0.2461(3) 0.7662(3) 0.42429(17) 0.0881(8) Uani 1 1 d D . . F5 F 0.1835(3) 0.5638(3) 0.4353(2) 0.0994(9) Uani 1 1 d D . . F6 F 0.4240(3) 0.7915(2) 0.5239(2) 0.1046(10) Uani 1 1 d D . . P2 P 0.07175(8) 0.26169(8) 0.12078(5) 0.04525(17) Uani 1 1 d D . . F7 F 0.0444(5) 0.1703(6) 0.0244(3) 0.0898(19) Uani 0.70 1 d PD A 1 F8 F 0.1038(6) 0.3847(5) 0.0870(4) 0.0833(17) Uani 0.70 1 d PD A 1 F9 F 0.1013(7) 0.3667(7) 0.2144(3) 0.0974(17) Uani 0.70 1 d PD A 1 F10 F 0.0410(9) 0.1434(7) 0.1509(7) 0.137(4) Uani 0.70 1 d PD A 1 F7A F 0.0490(14) 0.2075(16) 0.0205(5) 0.142(9) Uani 0.30 1 d PD A 2 F8A F 0.1146(10) 0.4041(9) 0.1233(11) 0.133(9) Uani 0.30 1 d PD A 2 F9A F 0.0859(15) 0.3047(19) 0.2218(5) 0.174(13) Uani 0.30 1 d PD A 2 F10A F 0.0262(15) 0.1133(13) 0.1183(13) 0.133(9) Uani 0.30 1 d PD A 2 F11 F -0.0811(2) 0.2910(3) 0.11574(18) 0.0842(7) Uani 1 1 d D A . F12 F 0.2241(2) 0.2373(3) 0.1246(2) 0.0926(8) Uani 1 1 d D A . N1S N 0.6495(3) 0.8328(3) 0.69085(19) 0.0544(6) Uani 1 1 d . . . O1S O 0.7279(4) 0.9114(3) 0.6780(3) 0.0941(10) Uani 1 1 d . . . O2S O 0.5665(3) 0.8654(3) 0.7373(2) 0.0796(8) Uani 1 1 d . . . C1S C 0.6524(5) 0.6901(4) 0.6475(3) 0.0653(10) Uani 1 1 d . . . H1SA H 0.577(6) 0.649(6) 0.652(4) 0.11(2) Uiso 1 1 d . . . H1SB H 0.638(5) 0.669(5) 0.589(4) 0.086(15) Uiso 1 1 d . . . H1SC H 0.737(6) 0.673(5) 0.660(3) 0.097(17) Uiso 1 1 d . . . N2S N 0.3030(5) 0.7973(4) 0.0465(2) 0.0854(12) Uani 1 1 d . . . O3S O 0.2422(6) 0.7197(4) 0.0748(3) 0.1318(18) Uani 1 1 d . . . O4S O 0.3832(5) 0.7667(6) 0.0029(3) 0.152(2) Uani 1 1 d . . . C2S C 0.2683(6) 0.9334(5) 0.0700(4) 0.0817(13) Uani 1 1 d . . . H2SA H 0.333(6) 0.995(7) 0.065(4) 0.12(2) Uiso 1 1 d . . . H2SB H 0.264(7) 0.950(7) 0.133(5) 0.14(2) Uiso 1 1 d . . . H2SC H 0.168(6) 0.938(6) 0.035(4) 0.111(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02659(11) 0.02708(11) 0.03101(11) 0.01196(7) 0.00689(7) 0.00332(7) S1 0.0349(3) 0.0328(3) 0.0381(3) 0.0102(2) 0.0062(2) -0.0014(2) S2 0.0388(3) 0.0421(3) 0.0376(3) 0.0187(3) 0.0025(2) 0.0039(2) N1 0.0385(11) 0.0315(10) 0.0391(11) 0.0139(8) 0.0128(8) 0.0076(8) C1 0.0321(13) 0.0482(15) 0.0636(18) 0.0174(13) 0.0161(12) 0.0005(11) C2 0.0327(13) 0.0472(15) 0.0578(17) 0.0178(13) 0.0140(12) 0.0098(11) C3 0.0644(18) 0.0421(14) 0.0384(13) 0.0129(11) 0.0215(12) 0.0152(13) C4 0.0664(19) 0.0411(14) 0.0341(13) 0.0079(11) 0.0038(12) 0.0027(13) C5 0.0591(18) 0.0434(14) 0.0408(14) 0.0225(11) 0.0137(12) 0.0090(12) C6 0.065(2) 0.0453(15) 0.0560(17) 0.0279(14) 0.0146(14) 0.0166(14) C7 0.0613(18) 0.0335(13) 0.0529(16) 0.0170(12) 0.0198(13) 0.0143(12) C8 0.0573(17) 0.0298(12) 0.0578(17) 0.0143(12) 0.0098(14) -0.0020(11) C9 0.0399(13) 0.0558(15) 0.0350(12) 0.0215(11) 0.0112(10) 0.0032(11) C10 0.0390(13) 0.0449(13) 0.0484(14) 0.0290(11) 0.0182(11) 0.0127(10) C11 0.0473(14) 0.0333(12) 0.0481(14) 0.0181(11) 0.0156(11) -0.0018(10) C12 0.0310(12) 0.0545(16) 0.0553(16) 0.0304(13) 0.0049(11) -0.0060(11) C13 0.0364(13) 0.0536(16) 0.0662(18) 0.0380(14) 0.0246(12) 0.0175(11) C14 0.0540(16) 0.0372(13) 0.0465(14) 0.0155(11) 0.0273(12) 0.0084(11) C15 0.066(2) 0.104(3) 0.0393(16) 0.0233(18) -0.0012(15) -0.002(2) C16 0.061(2) 0.070(2) 0.087(3) 0.054(2) 0.031(2) 0.0324(19) C17 0.103(4) 0.0351(16) 0.077(3) 0.0112(16) 0.029(2) -0.0074(18) C18 0.047(2) 0.107(4) 0.094(3) 0.054(3) -0.021(2) -0.028(2) C19 0.056(2) 0.102(3) 0.130(4) 0.083(3) 0.049(3) 0.049(2) C20 0.120(4) 0.0453(18) 0.067(2) 0.0068(17) 0.053(3) 0.011(2) P1 0.0410(4) 0.0419(4) 0.0493(4) 0.0127(3) 0.0112(3) 0.0056(3) F1 0.154(3) 0.0788(17) 0.172(3) 0.0370(19) 0.127(3) 0.0380(18) F2 0.0828(17) 0.0951(19) 0.140(3) 0.0785(19) 0.0095(16) 0.0187(14) F3 0.125(2) 0.0807(16) 0.0819(16) 0.0223(13) 0.0582(16) 0.0351(16) F4 0.106(2) 0.0977(19) 0.0746(15) 0.0456(14) 0.0113(14) 0.0302(16) F5 0.0676(15) 0.0698(15) 0.129(2) -0.0024(15) 0.0045(15) -0.0140(12) F6 0.0677(15) 0.0632(14) 0.167(3) 0.0378(17) -0.0231(17) -0.0133(12) P2 0.0490(4) 0.0442(4) 0.0437(4) 0.0126(3) 0.0120(3) 0.0135(3) F7 0.078(3) 0.092(3) 0.061(3) -0.028(2) 0.016(2) -0.003(2) F8 0.119(4) 0.067(3) 0.089(3) 0.045(3) 0.045(3) 0.028(3) F9 0.121(4) 0.106(3) 0.049(2) 0.000(2) 0.008(2) 0.042(3) F10 0.194(8) 0.103(5) 0.202(7) 0.116(6) 0.137(6) 0.069(5) F7A 0.139(14) 0.25(2) 0.070(8) 0.093(12) 0.044(8) -0.005(13) F8A 0.052(5) 0.029(4) 0.28(2) 0.001(8) 0.022(9) -0.009(3) F9A 0.163(17) 0.29(3) 0.037(5) -0.002(10) -0.015(7) 0.124(19) F10A 0.127(12) 0.068(7) 0.25(2) 0.070(10) 0.108(13) 0.035(7) F11 0.0507(12) 0.0963(18) 0.1012(18) 0.0201(14) 0.0208(12) 0.0204(11) F12 0.0579(13) 0.0917(18) 0.122(2) 0.0224(16) 0.0138(13) 0.0324(13) N1S 0.0558(15) 0.0437(13) 0.0584(16) 0.0139(12) -0.0007(12) 0.0052(11) O1S 0.093(2) 0.0629(17) 0.124(3) 0.0336(18) 0.015(2) -0.0152(16) O2S 0.083(2) 0.0776(18) 0.0729(17) 0.0110(14) 0.0213(15) 0.0220(15) C1S 0.068(2) 0.0449(17) 0.073(3) 0.0088(16) -0.0001(19) 0.0093(16) N2S 0.108(3) 0.077(2) 0.0533(18) 0.0069(17) -0.0208(19) 0.029(2) O3S 0.197(5) 0.083(2) 0.111(3) 0.050(2) -0.022(3) 0.005(3) O4S 0.126(4) 0.201(5) 0.087(3) -0.015(3) -0.005(2) 0.092(4) C2S 0.096(3) 0.055(2) 0.080(3) 0.009(2) -0.001(3) 0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.158(2) . ? Ru1 C13 2.219(3) . ? Ru1 C14 2.231(3) . ? Ru1 C10 2.234(2) . ? Ru1 C11 2.244(2) . ? Ru1 C12 2.258(3) . ? Ru1 C9 2.267(2) . ? Ru1 S2 2.3320(6) . ? Ru1 S1 2.3401(6) . ? S1 C1 1.820(3) . ? S1 C8 1.840(3) . ? S2 C4 1.817(3) . ? S2 C5 1.819(3) . ? N1 C2 1.493(4) . ? N1 C3 1.506(4) . ? C1 C2 1.501(4) . ? C3 C4 1.500(5) . ? C5 C6 1.510(4) . ? C6 C7 1.516(5) . ? C7 C8 1.516(5) . ? C9 C10 1.399(4) . ? C9 C14 1.435(4) . ? C9 C15 1.511(4) . ? C10 C11 1.428(4) . ? C10 C16 1.512(4) . ? C11 C12 1.398(4) . ? C11 C17 1.516(4) . ? C12 C13 1.430(5) . ? C12 C18 1.511(5) . ? C13 C14 1.405(5) . ? C13 C19 1.515(4) . ? C14 C20 1.506(4) . ? P1 F1 1.562(2) . ? P1 F2 1.572(2) . ? P1 F6 1.573(2) . ? P1 F5 1.577(2) . ? P1 F3 1.581(2) . ? P1 F4 1.589(2) . ? P2 F10 1.521(5) . ? P2 F8A 1.533(8) . ? P2 F7A 1.553(8) . ? P2 F7 1.559(3) . ? P2 F9A 1.571(9) . ? P2 F9 1.574(5) . ? P2 F12 1.580(2) . ? P2 F11 1.598(2) . ? P2 F10A 1.600(11) . ? P2 F8 1.607(4) . ? N1S O1S 1.201(4) . ? N1S O2S 1.215(4) . ? N1S C1S 1.467(4) . ? N2S O4S 1.160(6) . ? N2S O3S 1.239(6) . ? N2S C2S 1.459(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 C13 159.99(11) . . ? N1 Ru1 C14 152.80(10) . . ? C13 Ru1 C14 36.82(12) . . ? N1 Ru1 C10 92.51(9) . . ? C13 Ru1 C10 79.13(9) . . ? C14 Ru1 C10 66.67(10) . . ? N1 Ru1 C11 95.71(9) . . ? C13 Ru1 C11 66.67(10) . . ? C14 Ru1 C11 78.43(10) . . ? C10 Ru1 C11 37.18(11) . . ? N1 Ru1 C12 122.76(10) . . ? C13 Ru1 C12 37.24(12) . . ? C14 Ru1 C12 66.15(11) . . ? C10 Ru1 C12 66.08(10) . . ? C11 Ru1 C12 36.19(11) . . ? N1 Ru1 C9 116.20(9) . . ? C13 Ru1 C9 66.50(10) . . ? C14 Ru1 C9 37.20(10) . . ? C10 Ru1 C9 36.22(10) . . ? C11 Ru1 C9 65.71(10) . . ? C12 Ru1 C9 77.36(10) . . ? N1 Ru1 S2 83.72(6) . . ? C13 Ru1 S2 92.88(8) . . ? C14 Ru1 S2 123.39(8) . . ? C10 Ru1 S2 145.48(8) . . ? C11 Ru1 S2 108.87(8) . . ? C12 Ru1 S2 87.22(7) . . ? C9 Ru1 S2 159.30(7) . . ? N1 Ru1 S1 82.77(6) . . ? C13 Ru1 S1 117.24(9) . . ? C14 Ru1 S1 90.06(8) . . ? C10 Ru1 S1 114.52(8) . . ? C11 Ru1 S1 151.70(8) . . ? C12 Ru1 S1 154.36(9) . . ? C9 Ru1 S1 89.50(7) . . ? S2 Ru1 S1 99.08(2) . . ? C1 S1 C8 104.13(15) . . ? C1 S1 Ru1 101.62(10) . . ? C8 S1 Ru1 117.82(11) . . ? C4 S2 C5 99.93(15) . . ? C4 S2 Ru1 96.84(10) . . ? C5 S2 Ru1 116.59(11) . . ? C2 N1 C3 111.1(2) . . ? C2 N1 Ru1 111.33(16) . . ? C3 N1 Ru1 115.53(17) . . ? C2 C1 S1 107.89(19) . . ? N1 C2 C1 110.8(2) . . ? C4 C3 N1 111.4(2) . . ? C3 C4 S2 110.3(2) . . ? C6 C5 S2 112.0(2) . . ? C5 C6 C7 115.7(2) . . ? C8 C7 C6 115.2(3) . . ? C7 C8 S1 114.8(2) . . ? C10 C9 C14 119.9(3) . . ? C10 C9 C15 119.7(3) . . ? C14 C9 C15 120.4(3) . . ? C10 C9 Ru1 70.59(14) . . ? C14 C9 Ru1 70.04(15) . . ? C15 C9 Ru1 131.6(2) . . ? C9 C10 C11 119.9(2) . . ? C9 C10 C16 121.2(3) . . ? C11 C10 C16 118.8(3) . . ? C9 C10 Ru1 73.20(15) . . ? C11 C10 Ru1 71.79(14) . . ? C16 C10 Ru1 128.9(2) . . ? C12 C11 C10 120.1(2) . . ? C12 C11 C17 120.1(3) . . ? C10 C11 C17 119.8(3) . . ? C12 C11 Ru1 72.47(15) . . ? C10 C11 Ru1 71.03(14) . . ? C17 C11 Ru1 130.7(2) . . ? C11 C12 C13 120.2(3) . . ? C11 C12 C18 120.6(4) . . ? C13 C12 C18 119.1(3) . . ? C11 C12 Ru1 71.34(15) . . ? C13 C12 Ru1 69.89(14) . . ? C18 C12 Ru1 131.9(3) . . ? C14 C13 C12 119.5(2) . . ? C14 C13 C19 120.1(4) . . ? C12 C13 C19 120.3(4) . . ? C14 C13 Ru1 72.07(15) . . ? C12 C13 Ru1 72.87(15) . . ? C19 C13 Ru1 129.3(2) . . ? C13 C14 C9 120.0(3) . . ? C13 C14 C20 121.5(3) . . ? C9 C14 C20 118.5(4) . . ? C13 C14 Ru1 71.11(15) . . ? C9 C14 Ru1 72.75(14) . . ? C20 C14 Ru1 130.2(2) . . ? F1 P1 F2 90.05(19) . . ? F1 P1 F6 89.6(2) . . ? F2 P1 F6 92.79(16) . . ? F1 P1 F5 91.46(18) . . ? F2 P1 F5 87.13(17) . . ? F6 P1 F5 178.98(19) . . ? F1 P1 F3 178.57(19) . . ? F2 P1 F3 91.38(17) . . ? F6 P1 F3 90.41(18) . . ? F5 P1 F3 88.58(16) . . ? F1 P1 F4 91.65(18) . . ? F2 P1 F4 177.96(16) . . ? F6 P1 F4 88.34(16) . . ? F5 P1 F4 91.71(17) . . ? F3 P1 F4 86.92(15) . . ? F10 P2 F8A 160.7(8) . . ? F10 P2 F7A 106.7(8) . . ? F8A P2 F7A 92.6(7) . . ? F10 P2 F7 91.3(4) . . ? F8A P2 F7 107.9(7) . . ? F7A P2 F7 15.5(7) . . ? F10 P2 F9A 68.3(9) . . ? F8A P2 F9A 92.5(7) . . ? F7A P2 F9A 174.6(8) . . ? F7 P2 F9A 159.6(8) . . ? F10 P2 F9 94.7(5) . . ? F8A P2 F9 66.1(7) . . ? F7A P2 F9 158.4(7) . . ? F7 P2 F9 173.9(4) . . ? F9A P2 F9 26.4(8) . . ? F10 P2 F12 90.8(3) . . ? F8A P2 F12 88.0(4) . . ? F7A P2 F12 90.3(5) . . ? F7 P2 F12 88.6(2) . . ? F9A P2 F12 91.8(5) . . ? F9 P2 F12 91.8(3) . . ? F10 P2 F11 91.3(3) . . ? F8A P2 F11 90.0(4) . . ? F7A P2 F11 89.1(5) . . ? F7 P2 F11 91.4(2) . . ? F9A P2 F11 89.0(5) . . ? F9 P2 F11 88.0(3) . . ? F12 P2 F11 177.87(17) . . ? F10 P2 F10A 19.2(9) . . ? F8A P2 F10A 179.6(7) . . ? F7A P2 F10A 87.5(7) . . ? F7 P2 F10A 72.2(8) . . ? F9A P2 F10A 87.4(7) . . ? F9 P2 F10A 113.8(8) . . ? F12 P2 F10A 92.4(5) . . ? F11 P2 F10A 89.6(5) . . ? F10 P2 F8 178.9(4) . . ? F8A P2 F8 20.4(7) . . ? F7A P2 F8 72.1(6) . . ? F7 P2 F8 87.5(3) . . ? F9A P2 F8 112.9(8) . . ? F9 P2 F8 86.4(3) . . ? F12 P2 F8 89.1(3) . . ? F11 P2 F8 88.8(3) . . ? F10A P2 F8 159.6(7) . . ? O1S N1S O2S 123.3(3) . . ? O1S N1S C1S 118.6(4) . . ? O2S N1S C1S 118.0(3) . . ? O4S N2S O3S 123.5(5) . . ? O4S N2S C2S 119.9(6) . . ? O3S N2S C2S 116.6(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.629 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.085 #===END Complex 6 data_3025a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H36 F6 I N2 O2 P Ru S2' _chemical_formula_weight 761.56 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.9370(10) _cell_length_b 16.8727(10) _cell_length_c 19.7224(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5636.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3442 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 22.78 _exptl_crystal_description Plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3024 _exptl_absorpt_coefficient_mu 1.916 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.5297 _exptl_absorpt_correction_T_max 0.9273 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30654 _diffrn_reflns_av_R_equivalents 0.0761 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4948 _reflns_number_gt 3970 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0418P)^2^+24.1498P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4948 _refine_ls_number_parameters 320 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1151 _refine_ls_goodness_of_fit_ref 1.138 _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 0.06474(3) 0.32962(3) 0.36471(3) 0.01664(15) Uani 1 1 d . . . I I 0.13670(3) 0.75433(3) 0.38417(3) 0.03783(17) Uani 1 1 d . . . S1 S 0.08405(10) 0.46344(9) 0.39287(9) 0.0243(4) Uani 1 1 d . . . S2 S 0.03690(12) 0.33478(10) 0.24861(9) 0.0309(4) Uani 1 1 d . . . N1 N 0.1844(3) 0.3388(4) 0.3296(3) 0.0294(14) Uani 1 1 d . . . H1 H 0.202(6) 0.298(6) 0.352(5) 0.08(3) Uiso 1 1 d . . . C1 C 0.0719(4) 0.5367(4) 0.3275(4) 0.0328(18) Uani 1 1 d . . . H1A H 0.0911 0.5875 0.3437 0.049 Uiso 1 1 calc R . . H1B H 0.0164 0.5412 0.3159 0.049 Uiso 1 1 calc R . . H1C H 0.1017 0.5210 0.2877 0.049 Uiso 1 1 calc R . . C2 C 0.1903(5) 0.4607(5) 0.3973(5) 0.044(2) Uani 1 1 d . . . H2A H 0.2113 0.5148 0.3986 0.053 Uiso 1 1 calc R . . H2B H 0.2069 0.4332 0.4387 0.053 Uiso 1 1 calc R . . C3 C 0.2214(4) 0.4186(4) 0.3372(5) 0.044(2) Uani 1 1 d . . . H3A H 0.2787 0.4126 0.3416 0.053 Uiso 1 1 calc R . . H3B H 0.2108 0.4501 0.2965 0.053 Uiso 1 1 calc R . . C4 C 0.1921(5) 0.3082(5) 0.2586(4) 0.046(2) Uani 1 1 d . . . H4A H 0.1828 0.2509 0.2583 0.055 Uiso 1 1 calc R . . H4B H 0.2459 0.3177 0.2423 0.055 Uiso 1 1 calc R . . C5 C 0.1344(5) 0.3478(6) 0.2119(4) 0.052(2) Uani 1 1 d . . . H5A H 0.1367 0.3237 0.1668 0.062 Uiso 1 1 calc R . . H5B H 0.1468 0.4044 0.2077 0.062 Uiso 1 1 calc R . . C6 C -0.0176(5) 0.4170(5) 0.2142(5) 0.052(2) Uani 1 1 d . . . H6A H 0.0153 0.4640 0.2144 0.078 Uiso 1 1 calc R . . H6B H -0.0643 0.4263 0.2416 0.078 Uiso 1 1 calc R . . H6C H -0.0334 0.4049 0.1681 0.078 Uiso 1 1 calc R . . C7 C 0.0789(4) 0.2059(3) 0.4005(4) 0.0232(14) Uani 1 1 d U . . C8 C 0.0080(4) 0.2093(4) 0.3630(4) 0.0252(15) Uani 1 1 d U . . C9 C -0.0494(4) 0.2687(4) 0.3800(3) 0.0217(15) Uani 1 1 d . . . C10 C -0.0377(4) 0.3202(4) 0.4343(3) 0.0199(14) Uani 1 1 d . . . C11 C 0.0323(4) 0.3109(3) 0.4751(3) 0.0202(15) Uani 1 1 d . . . C12 C 0.0909(4) 0.2562(4) 0.4570(3) 0.0215(14) Uani 1 1 d U . . C13 C 0.1412(5) 0.1429(4) 0.3820(4) 0.040(2) Uani 1 1 d . . . H13A H 0.1371 0.1303 0.3341 0.060 Uiso 1 1 calc R . . H13B H 0.1321 0.0954 0.4086 0.060 Uiso 1 1 calc R . . H13C H 0.1935 0.1634 0.3916 0.060 Uiso 1 1 calc R . . C14 C -0.0088(5) 0.1526(4) 0.3048(4) 0.0364(19) Uani 1 1 d . . . H14A H 0.0370 0.1193 0.2970 0.055 Uiso 1 1 calc R . . H14B H -0.0204 0.1827 0.2640 0.055 Uiso 1 1 calc R . . H14C H -0.0538 0.1196 0.3162 0.055 Uiso 1 1 calc R . . C15 C -0.1245(4) 0.2747(5) 0.3379(4) 0.0364(19) Uani 1 1 d . . . H15A H -0.1644 0.2399 0.3567 0.055 Uiso 1 1 calc R . . H15B H -0.1133 0.2591 0.2915 0.055 Uiso 1 1 calc R . . H15C H -0.1435 0.3289 0.3386 0.055 Uiso 1 1 calc R . . C16 C -0.0986(4) 0.3815(4) 0.4543(4) 0.0298(17) Uani 1 1 d . . . H16A H -0.0722 0.4296 0.4686 0.045 Uiso 1 1 calc R . . H16B H -0.1304 0.3611 0.4913 0.045 Uiso 1 1 calc R . . H16C H -0.1324 0.3929 0.4157 0.045 Uiso 1 1 calc R . . C17 C 0.0435(4) 0.3635(4) 0.5365(4) 0.0286(16) Uani 1 1 d . . . H17A H 0.0292 0.3344 0.5771 0.043 Uiso 1 1 calc R . . H17B H 0.0103 0.4100 0.5323 0.043 Uiso 1 1 calc R . . H17C H 0.0984 0.3797 0.5395 0.043 Uiso 1 1 calc R . . C18 C 0.1653(4) 0.2465(4) 0.5000(4) 0.0345(17) Uani 1 1 d . . . H18A H 0.1746 0.2947 0.5256 0.052 Uiso 1 1 calc R . . H18B H 0.2101 0.2361 0.4707 0.052 Uiso 1 1 calc R . . H18C H 0.1584 0.2025 0.5311 0.052 Uiso 1 1 calc R . . P1 P 0.28548(12) 0.55709(11) 0.16901(11) 0.0331(5) Uani 1 1 d . . . F1 F 0.2803(4) 0.5681(4) 0.2471(3) 0.091(2) Uani 1 1 d . . . F2 F 0.1918(3) 0.5549(4) 0.1660(3) 0.0833(19) Uani 1 1 d . . . F3 F 0.2891(3) 0.5456(4) 0.0890(3) 0.0689(16) Uani 1 1 d . . . F4 F 0.3770(3) 0.5556(5) 0.1696(4) 0.099(3) Uani 1 1 d . . . F5 F 0.2834(4) 0.4641(3) 0.1786(3) 0.080(2) Uani 1 1 d . . . F6 F 0.2864(4) 0.6484(3) 0.1565(4) 0.093(2) Uani 1 1 d . . . N1S N 0.0850(7) 0.5063(6) 0.0439(5) 0.079(3) Uani 1 1 d . . . C1S C 0.1132(6) 0.5784(6) 0.0124(6) 0.071(3) Uani 1 1 d . . . H1S1 H 0.1703 0.5809 0.0161 0.107 Uiso 1 1 calc R . . H1S2 H 0.0901 0.6239 0.0351 0.107 Uiso 1 1 calc R . . H1S3 H 0.0982 0.5788 -0.0351 0.107 Uiso 1 1 calc R . . O1S O 0.0222(7) 0.5177(6) 0.0768(5) 0.118(4) Uani 1 1 d . . . O2S O 0.1156(9) 0.4466(6) 0.0390(6) 0.180(7) 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 0.0186(3) 0.0126(2) 0.0188(3) 0.0003(2) 0.0012(2) -0.0018(2) I 0.0316(3) 0.0338(3) 0.0481(3) 0.0055(2) -0.0028(2) -0.0097(2) S1 0.0306(10) 0.0151(8) 0.0272(10) -0.0022(7) 0.0022(7) -0.0046(7) S2 0.0465(11) 0.0253(9) 0.0210(10) 0.0033(8) -0.0033(8) -0.0076(8) N1 0.026(3) 0.031(3) 0.031(4) 0.015(3) 0.007(3) 0.005(3) C1 0.036(4) 0.016(3) 0.046(5) 0.004(3) 0.004(4) -0.001(3) C2 0.043(5) 0.030(4) 0.059(6) 0.007(4) -0.021(4) -0.012(4) C3 0.014(4) 0.029(4) 0.087(7) 0.025(4) -0.004(4) -0.003(3) C4 0.047(5) 0.054(5) 0.038(5) 0.001(4) 0.024(4) 0.011(4) C5 0.059(6) 0.078(7) 0.018(4) 0.006(4) 0.021(4) 0.000(5) C6 0.063(6) 0.047(5) 0.046(6) 0.014(4) -0.025(5) -0.004(5) C7 0.034(3) 0.006(3) 0.030(3) 0.002(3) 0.003(3) -0.009(2) C8 0.037(4) 0.014(3) 0.025(4) -0.001(3) 0.002(3) -0.011(3) C9 0.019(3) 0.023(3) 0.023(4) 0.004(3) 0.000(3) -0.011(3) C10 0.021(3) 0.019(3) 0.020(4) 0.006(3) 0.003(3) -0.005(3) C11 0.028(4) 0.009(3) 0.023(4) 0.002(3) 0.003(3) -0.006(3) C12 0.023(3) 0.015(3) 0.026(4) 0.006(3) 0.002(3) -0.002(3) C13 0.054(5) 0.021(4) 0.045(5) -0.002(3) 0.002(4) 0.008(4) C14 0.056(5) 0.018(4) 0.036(5) -0.010(3) -0.012(4) -0.010(3) C15 0.025(4) 0.042(4) 0.043(5) 0.002(4) -0.011(3) -0.012(3) C16 0.027(4) 0.032(4) 0.031(4) 0.001(3) 0.002(3) 0.011(3) C17 0.026(4) 0.032(4) 0.027(4) -0.008(3) 0.002(3) -0.002(3) C18 0.033(4) 0.038(4) 0.032(4) 0.006(4) -0.003(3) 0.005(4) P1 0.0290(11) 0.0308(10) 0.0396(12) 0.0049(9) 0.0080(9) -0.0001(9) F1 0.125(6) 0.106(5) 0.041(4) -0.006(3) 0.013(3) -0.057(4) F2 0.035(3) 0.120(5) 0.095(5) 0.002(4) 0.013(3) 0.002(3) F3 0.074(4) 0.087(4) 0.045(3) 0.000(3) 0.010(3) -0.010(3) F4 0.027(3) 0.165(7) 0.104(5) 0.067(5) -0.005(3) -0.010(4) F5 0.099(5) 0.037(3) 0.104(5) 0.012(3) 0.059(4) 0.006(3) F6 0.141(6) 0.033(3) 0.106(5) 0.011(3) 0.048(5) 0.004(3) N1S 0.113(9) 0.075(7) 0.050(6) -0.018(5) -0.012(6) 0.003(6) C1S 0.068(7) 0.068(7) 0.078(8) 0.015(6) 0.020(6) -0.011(6) O1S 0.162(10) 0.124(8) 0.067(6) -0.018(6) 0.038(6) -0.055(7) O2S 0.344(18) 0.065(6) 0.131(10) -0.037(6) -0.089(11) 0.077(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.147(6) . ? Ru1 C9 2.211(6) . ? Ru1 C7 2.217(6) . ? Ru1 C10 2.218(6) . ? Ru1 C8 2.245(6) . ? Ru1 C12 2.246(6) . ? Ru1 C11 2.268(7) . ? Ru1 S2 2.3394(19) . ? Ru1 S1 2.3480(17) . ? S1 C1 1.797(7) . ? S1 C2 1.802(8) . ? S2 C6 1.799(8) . ? S2 C5 1.816(8) . ? N1 C3 1.492(9) . ? N1 C4 1.499(10) . ? C2 C3 1.479(12) . ? C4 C5 1.499(12) . ? C7 C8 1.412(10) . ? C7 C12 1.415(9) . ? C7 C13 1.540(10) . ? C8 C9 1.436(10) . ? C8 C14 1.522(9) . ? C9 C10 1.393(9) . ? C9 C15 1.522(9) . ? C10 C11 1.443(9) . ? C10 C16 1.513(9) . ? C11 C12 1.402(9) . ? C11 C17 1.513(9) . ? C12 C18 1.527(9) . ? P1 F4 1.550(5) . ? P1 F1 1.554(6) . ? P1 F6 1.560(5) . ? P1 F5 1.580(5) . ? P1 F2 1.588(5) . ? P1 F3 1.591(6) . ? N1S O2S 1.136(12) . ? N1S O1S 1.260(13) . ? N1S C1S 1.448(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 N1 Ru1 C9 154.6(2) . . ? N1 Ru1 C7 93.9(2) . . ? C9 Ru1 C7 67.3(2) . . ? N1 Ru1 C10 160.6(2) . . ? C9 Ru1 C10 36.7(2) . . ? C7 Ru1 C10 79.7(2) . . ? N1 Ru1 C8 117.6(2) . . ? C9 Ru1 C8 37.6(2) . . ? C7 Ru1 C8 36.9(2) . . ? C10 Ru1 C8 67.1(2) . . ? N1 Ru1 C12 96.6(2) . . ? C9 Ru1 C12 78.8(2) . . ? C7 Ru1 C12 37.0(2) . . ? C10 Ru1 C12 67.3(2) . . ? C8 Ru1 C12 66.3(2) . . ? N1 Ru1 C11 123.2(2) . . ? C9 Ru1 C11 66.0(2) . . ? C7 Ru1 C11 65.7(2) . . ? C10 Ru1 C11 37.5(2) . . ? C8 Ru1 C11 77.6(2) . . ? C12 Ru1 C11 36.2(2) . . ? N1 Ru1 S2 82.67(18) . . ? C9 Ru1 S2 88.53(17) . . ? C7 Ru1 S2 111.64(19) . . ? C10 Ru1 S2 116.76(18) . . ? C8 Ru1 S2 86.12(19) . . ? C12 Ru1 S2 148.58(17) . . ? C11 Ru1 S2 153.66(17) . . ? N1 Ru1 S1 82.85(18) . . ? C9 Ru1 S1 122.48(18) . . ? C7 Ru1 S1 144.60(19) . . ? C10 Ru1 S1 91.81(17) . . ? C8 Ru1 S1 158.79(19) . . ? C12 Ru1 S1 108.15(17) . . ? C11 Ru1 S1 86.60(15) . . ? S2 Ru1 S1 102.93(6) . . ? C1 S1 C2 99.6(4) . . ? C1 S1 Ru1 118.4(3) . . ? C2 S1 Ru1 97.2(3) . . ? C6 S2 C5 102.9(4) . . ? C6 S2 Ru1 120.1(3) . . ? C5 S2 Ru1 102.2(3) . . ? C3 N1 C4 111.5(6) . . ? C3 N1 Ru1 115.4(5) . . ? C4 N1 Ru1 111.0(5) . . ? C3 C2 S1 109.2(5) . . ? C2 C3 N1 111.3(6) . . ? N1 C4 C5 111.3(6) . . ? C4 C5 S2 107.1(6) . . ? C8 C7 C12 120.7(6) . . ? C8 C7 C13 119.1(6) . . ? C12 C7 C13 120.2(6) . . ? C8 C7 Ru1 72.6(4) . . ? C12 C7 Ru1 72.7(3) . . ? C13 C7 Ru1 130.4(5) . . ? C7 C8 C9 118.9(6) . . ? C7 C8 C14 121.9(6) . . ? C9 C8 C14 119.2(6) . . ? C7 C8 Ru1 70.5(3) . . ? C9 C8 Ru1 69.9(3) . . ? C14 C8 Ru1 131.3(5) . . ? C10 C9 C8 121.2(6) . . ? C10 C9 C15 119.7(6) . . ? C8 C9 C15 119.0(6) . . ? C10 C9 Ru1 71.9(4) . . ? C8 C9 Ru1 72.5(4) . . ? C15 C9 Ru1 128.7(5) . . ? C9 C10 C11 118.5(6) . . ? C9 C10 C16 122.0(6) . . ? C11 C10 C16 119.3(6) . . ? C9 C10 Ru1 71.4(4) . . ? C11 C10 Ru1 73.1(4) . . ? C16 C10 Ru1 130.2(4) . . ? C12 C11 C10 120.8(6) . . ? C12 C11 C17 120.1(6) . . ? C10 C11 C17 119.1(6) . . ? C12 C11 Ru1 71.1(4) . . ? C10 C11 Ru1 69.4(4) . . ? C17 C11 Ru1 131.0(4) . . ? C11 C12 C7 119.6(6) . . ? C11 C12 C18 120.8(6) . . ? C7 C12 C18 119.4(6) . . ? C11 C12 Ru1 72.7(4) . . ? C7 C12 Ru1 70.4(4) . . ? C18 C12 Ru1 132.2(5) . . ? F4 P1 F1 93.0(4) . . ? F4 P1 F6 90.5(4) . . ? F1 P1 F6 92.3(4) . . ? F4 P1 F5 90.3(4) . . ? F1 P1 F5 89.9(4) . . ? F6 P1 F5 177.6(4) . . ? F4 P1 F2 177.1(4) . . ? F1 P1 F2 89.0(4) . . ? F6 P1 F2 91.5(4) . . ? F5 P1 F2 87.6(3) . . ? F4 P1 F3 88.1(4) . . ? F1 P1 F3 178.9(3) . . ? F6 P1 F3 87.9(4) . . ? F5 P1 F3 89.9(3) . . ? F2 P1 F3 89.9(3) . . ? O2S N1S O1S 124.4(14) . . ? O2S N1S C1S 123.9(14) . . ? O1S N1S C1S 111.8(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.809 _refine_diff_density_min -1.230 _refine_diff_density_rms 0.136 #===END Complex 7 data_2109 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H32 F6 N P Ru S2' _chemical_formula_weight 584.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.0476(5) _cell_length_b 18.5151(9) _cell_length_c 24.9301(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4637.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5248 _cell_measurement_theta_min 2.446 _cell_measurement_theta_max 27.987 _exptl_crystal_description BLOCK _exptl_crystal_colour Orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 0.980 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31086 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5321 _reflns_number_gt 4472 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0359P)^2^+5.0595P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5321 _refine_ls_number_parameters 405 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.0992 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.197 _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 0.33779(3) 0.796751(14) 0.624268(10) 0.01662(9) Uani 1 1 d . . . S1 S 0.29087(10) 0.79520(6) 0.53066(4) 0.0311(2) Uani 1 1 d . . . S2 S 0.50383(10) 0.70904(5) 0.62031(4) 0.0312(2) Uani 1 1 d . A . N1 N 0.4919(3) 0.86753(16) 0.59624(12) 0.0230(6) Uani 1 1 d . . . H1 H 0.514(3) 0.8938(19) 0.6200(13) 0.010(9) Uiso 1 1 d . . . C1 C 0.3864(6) 0.8722(3) 0.50678(18) 0.0429(11) Uani 1 1 d . . . H1A H 0.460(5) 0.858(2) 0.4866(18) 0.047(14) Uiso 1 1 d . . . H1B H 0.333(5) 0.899(3) 0.482(2) 0.065(17) Uiso 1 1 d . . . C2 C 0.4400(5) 0.9159(2) 0.55305(17) 0.0332(9) Uani 1 1 d . . . H2A H 0.508(4) 0.946(2) 0.5404(16) 0.034(11) Uiso 1 1 d . . . H2B H 0.376(5) 0.942(2) 0.5687(17) 0.038(12) Uiso 1 1 d . . . C3 C 0.6142(4) 0.8300(3) 0.5785(2) 0.0398(11) Uani 1 1 d . . . H3A H 0.679(4) 0.861(2) 0.5806(14) 0.018(10) Uiso 1 1 d . . . H3B H 0.597(4) 0.812(2) 0.5407(17) 0.034(11) Uiso 1 1 d . . . C4 C 0.6455(4) 0.7686(3) 0.6150(2) 0.0436(12) Uani 1 1 d . . . H4A H 0.662(5) 0.784(3) 0.650(2) 0.047(14) Uiso 1 1 d . . . H4B H 0.714(5) 0.744(3) 0.604(2) 0.048(14) Uiso 1 1 d . . . C5 C 0.5173(5) 0.6604(2) 0.5572(2) 0.0394(11) Uani 1 1 d . . . H5A H 0.500(4) 0.688(2) 0.5303(17) 0.030(12) Uiso 1 1 d . . . H5B H 0.594(5) 0.643(3) 0.5567(18) 0.045(14) Uiso 1 1 d . . . C6 C 0.4377(9) 0.5946(5) 0.5622(4) 0.0383(19) Uani 0.60 1 d P A 1 H6A H 0.4636 0.5589 0.5862 0.046 Uiso 0.60 1 calc PR A 1 C6A C 0.3880(19) 0.6166(7) 0.5419(6) 0.040(3) Uani 0.40 1 d P A 2 H6AA H 0.3077 0.6416 0.5410 0.048 Uiso 0.40 1 calc PR A 2 C7 C 0.3337(13) 0.5858(8) 0.5340(5) 0.064(3) Uani 0.60 1 d P A 1 H7A H 0.3073 0.6214 0.5099 0.077 Uiso 0.60 1 calc PR A 1 H7B H 0.2838 0.5438 0.5375 0.077 Uiso 0.60 1 calc PR A 1 C7A C 0.386(2) 0.5488(8) 0.5307(6) 0.060(4) Uani 0.40 1 d P A 2 H7AA H 0.4643 0.5221 0.5313 0.072 Uiso 0.40 1 calc PR A 2 H7AB H 0.3058 0.5264 0.5220 0.072 Uiso 0.40 1 calc PR A 2 C8 C 0.3111(4) 0.7683(2) 0.71122(14) 0.0249(8) Uani 1 1 d . . . C9 C 0.3195(4) 0.8440(2) 0.70573(14) 0.0254(8) Uani 1 1 d . . . C10 C 0.2269(4) 0.88140(19) 0.67147(14) 0.0252(8) Uani 1 1 d . . . C11 C 0.1326(3) 0.8419(2) 0.64131(15) 0.0253(8) Uani 1 1 d . . . C12 C 0.1333(3) 0.7643(2) 0.64285(15) 0.0244(8) Uani 1 1 d . . . C13 C 0.2191(4) 0.72812(19) 0.67909(14) 0.0241(8) Uani 1 1 d . . . C14 C 0.3985(6) 0.7287(3) 0.7506(2) 0.0450(12) Uani 1 1 d . . . H14A H 0.451(7) 0.762(4) 0.767(3) 0.09(2) Uiso 1 1 d . . . H14B H 0.343(6) 0.711(3) 0.779(3) 0.08(2) Uiso 1 1 d . . . H14C H 0.433(6) 0.693(3) 0.736(2) 0.056(18) Uiso 1 1 d . . . C15 C 0.4204(5) 0.8865(3) 0.73726(19) 0.0403(11) Uani 1 1 d . . . H15A H 0.489(6) 0.862(3) 0.745(2) 0.064(18) Uiso 1 1 d . . . H15B H 0.389(5) 0.896(3) 0.769(2) 0.066(17) Uiso 1 1 d . . . H15C H 0.446(5) 0.932(3) 0.723(2) 0.068(17) Uiso 1 1 d . . . C16 C 0.2281(7) 0.9630(2) 0.6702(2) 0.0450(12) Uani 1 1 d . . . H16A H 0.308(6) 0.980(3) 0.664(2) 0.07(2) Uiso 1 1 d . . . H16B H 0.185(7) 0.979(4) 0.642(3) 0.10(3) Uiso 1 1 d . . . H16C H 0.193(6) 0.980(3) 0.701(3) 0.08(2) Uiso 1 1 d . . . C17 C 0.0339(6) 0.8802(4) 0.6061(3) 0.0464(12) Uani 1 1 d . . . H17A H 0.058(5) 0.883(3) 0.573(2) 0.059(17) Uiso 1 1 d . . . H17B H 0.017(6) 0.923(4) 0.614(2) 0.09(2) Uiso 1 1 d . . . H17C H -0.028(6) 0.857(4) 0.606(3) 0.08(2) Uiso 1 1 d . . . C18 C 0.0400(5) 0.7221(3) 0.6076(2) 0.0386(11) Uani 1 1 d . . . H18A H 0.018(4) 0.745(2) 0.5763(18) 0.038(13) Uiso 1 1 d . . . H18B H -0.029(6) 0.712(3) 0.626(2) 0.054(16) Uiso 1 1 d . . . H18C H 0.069(6) 0.682(3) 0.593(2) 0.068(18) Uiso 1 1 d . . . C19 C 0.2128(6) 0.6470(2) 0.6849(2) 0.0400(11) Uani 1 1 d . . . H19A H 0.180(6) 0.634(4) 0.714(3) 0.09(2) Uiso 1 1 d . . . H19B H 0.292(7) 0.625(3) 0.686(2) 0.08(2) Uiso 1 1 d . . . H19C H 0.162(6) 0.626(4) 0.661(3) 0.09(2) Uiso 1 1 d . . . P1 P 0.79350(11) 0.52925(5) 0.65304(4) 0.0306(2) Uani 1 1 d . . . F1 F 0.6454(3) 0.53051(16) 0.67368(15) 0.0759(11) Uani 1 1 d . . . F2 F 0.7856(3) 0.61259(13) 0.63774(12) 0.0528(7) Uani 1 1 d . . . F3 F 0.9430(3) 0.52628(14) 0.63213(12) 0.0537(7) Uani 1 1 d . . . F4 F 0.8044(3) 0.44481(13) 0.66806(11) 0.0510(7) Uani 1 1 d . . . F5 F 0.7444(3) 0.50685(16) 0.59482(12) 0.0634(8) Uani 1 1 d . . . F6 F 0.8457(4) 0.54920(18) 0.71077(12) 0.0741(10) 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 0.01613(14) 0.01684(14) 0.01690(14) -0.00052(10) -0.00086(10) 0.00095(10) S1 0.0351(5) 0.0382(5) 0.0202(4) -0.0009(4) -0.0066(4) -0.0043(4) S2 0.0287(5) 0.0278(5) 0.0370(5) 0.0042(4) 0.0059(4) 0.0102(4) N1 0.0249(16) 0.0212(15) 0.0229(15) -0.0068(12) 0.0019(13) -0.0057(12) C1 0.058(3) 0.044(3) 0.027(2) 0.0056(19) 0.002(2) -0.012(2) C2 0.044(3) 0.025(2) 0.031(2) 0.0060(16) 0.0036(19) -0.0061(19) C3 0.022(2) 0.035(2) 0.062(3) -0.012(2) 0.012(2) -0.0105(19) C4 0.019(2) 0.047(3) 0.065(3) -0.009(2) -0.002(2) 0.0066(19) C5 0.041(3) 0.029(2) 0.048(3) -0.007(2) 0.022(2) 0.006(2) C6 0.051(5) 0.021(4) 0.043(5) 0.010(3) -0.007(4) 0.001(4) C6A 0.063(10) 0.023(7) 0.033(7) 0.001(6) 0.014(7) -0.001(7) C7 0.088(10) 0.041(7) 0.064(7) 0.014(6) -0.023(6) -0.022(6) C7A 0.087(12) 0.029(8) 0.063(9) 0.003(7) 0.022(8) -0.010(8) C8 0.0263(19) 0.0312(19) 0.0173(17) 0.0001(14) 0.0038(14) 0.0029(16) C9 0.0247(19) 0.0293(19) 0.0222(17) -0.0029(15) 0.0051(14) -0.0032(15) C10 0.028(2) 0.0227(18) 0.0244(18) -0.0020(14) 0.0098(15) 0.0020(15) C11 0.0186(18) 0.030(2) 0.0271(18) 0.0045(15) 0.0048(14) 0.0075(15) C12 0.0166(18) 0.032(2) 0.0240(17) -0.0022(15) 0.0039(14) -0.0028(15) C13 0.0274(19) 0.0212(17) 0.0238(18) 0.0028(14) 0.0078(15) -0.0001(15) C14 0.052(3) 0.056(3) 0.027(2) 0.012(2) -0.009(2) 0.008(3) C15 0.045(3) 0.043(3) 0.033(2) -0.012(2) -0.004(2) -0.011(2) C16 0.069(4) 0.018(2) 0.048(3) -0.0025(19) 0.012(3) 0.002(2) C17 0.037(3) 0.048(3) 0.054(3) 0.007(3) -0.008(2) 0.019(3) C18 0.025(2) 0.047(3) 0.044(3) -0.005(2) -0.004(2) -0.015(2) C19 0.053(3) 0.022(2) 0.045(3) 0.0041(19) 0.006(2) -0.004(2) P1 0.0310(5) 0.0239(5) 0.0368(6) 0.0017(4) 0.0054(4) 0.0031(4) F1 0.0514(19) 0.0489(18) 0.127(3) 0.0148(19) 0.0449(19) 0.0104(14) F2 0.0505(16) 0.0258(13) 0.082(2) 0.0128(13) 0.0057(14) 0.0038(12) F3 0.0354(14) 0.0477(16) 0.078(2) -0.0050(14) 0.0155(13) 0.0012(12) F4 0.0605(17) 0.0278(13) 0.0646(18) 0.0079(12) 0.0173(14) 0.0114(12) F5 0.076(2) 0.0600(19) 0.0539(18) -0.0001(14) -0.0262(16) -0.0178(16) F6 0.119(3) 0.061(2) 0.0420(17) -0.0107(14) -0.0110(17) 0.0159(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.145(3) . ? Ru1 C12 2.190(4) . ? Ru1 C13 2.215(3) . ? Ru1 C9 2.219(3) . ? Ru1 C8 2.247(3) . ? Ru1 C10 2.255(3) . ? Ru1 C11 2.265(3) . ? Ru1 S2 2.3303(10) . ? Ru1 S1 2.3809(9) . ? S1 C1 1.819(5) . ? S2 C4 1.805(5) . ? S2 C5 1.818(5) . ? N1 C3 1.479(5) . ? N1 C2 1.494(5) . ? C1 C2 1.508(6) . ? C3 C4 1.490(7) . ? C5 C6 1.461(9) . ? C5 C6A 1.578(19) . ? C6 C7 1.270(15) . ? C6A C7A 1.286(19) . ? C8 C9 1.411(5) . ? C8 C13 1.432(5) . ? C8 C14 1.507(6) . ? C9 C10 1.440(5) . ? C9 C15 1.505(6) . ? C10 C11 1.413(5) . ? C10 C16 1.512(5) . ? C11 C12 1.438(5) . ? C11 C17 1.502(6) . ? C12 C13 1.417(5) . ? C12 C18 1.503(6) . ? C13 C19 1.511(5) . ? P1 F1 1.575(3) . ? P1 F6 1.576(3) . ? P1 F5 1.588(3) . ? P1 F3 1.591(3) . ? P1 F2 1.592(3) . ? P1 F4 1.611(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 N1 Ru1 C12 156.00(13) . . ? N1 Ru1 C13 160.07(13) . . ? C12 Ru1 C13 37.51(14) . . ? N1 Ru1 C9 96.72(13) . . ? C12 Ru1 C9 80.61(13) . . ? C13 Ru1 C9 67.47(13) . . ? N1 Ru1 C8 122.94(13) . . ? C12 Ru1 C8 67.64(13) . . ? C13 Ru1 C8 37.42(13) . . ? C9 Ru1 C8 36.84(14) . . ? N1 Ru1 C10 95.86(12) . . ? C12 Ru1 C10 67.46(14) . . ? C13 Ru1 C10 79.07(13) . . ? C9 Ru1 C10 37.54(13) . . ? C8 Ru1 C10 66.45(13) . . ? N1 Ru1 C11 119.50(13) . . ? C12 Ru1 C11 37.61(14) . . ? C13 Ru1 C11 66.79(13) . . ? C9 Ru1 C11 66.87(13) . . ? C8 Ru1 C11 78.29(13) . . ? C10 Ru1 C11 36.44(14) . . ? N1 Ru1 S2 83.98(9) . . ? C12 Ru1 S2 119.29(11) . . ? C13 Ru1 S2 90.68(10) . . ? C9 Ru1 S2 111.90(10) . . ? C8 Ru1 S2 87.87(10) . . ? C10 Ru1 S2 149.36(10) . . ? C11 Ru1 S2 156.48(10) . . ? N1 Ru1 S1 80.27(9) . . ? C12 Ru1 S1 91.05(10) . . ? C13 Ru1 S1 119.42(10) . . ? C9 Ru1 S1 152.29(10) . . ? C8 Ru1 S1 156.79(10) . . ? C10 Ru1 S1 114.97(10) . . ? C11 Ru1 S1 90.46(10) . . ? S2 Ru1 S1 95.27(4) . . ? C1 S1 Ru1 101.94(15) . . ? C4 S2 C5 100.4(2) . . ? C4 S2 Ru1 98.18(16) . . ? C5 S2 Ru1 115.81(19) . . ? C3 N1 C2 110.9(3) . . ? C3 N1 Ru1 114.2(2) . . ? C2 N1 Ru1 110.4(2) . . ? C2 C1 S1 111.0(3) . . ? N1 C2 C1 110.8(3) . . ? N1 C3 C4 110.6(4) . . ? C3 C4 S2 110.1(3) . . ? C6 C5 C6A 31.0(5) . . ? C6 C5 S2 107.4(4) . . ? C6A C5 S2 113.7(5) . . ? C7 C6 C5 120.7(11) . . ? C7A C6A C5 124.6(16) . . ? C9 C8 C13 120.0(3) . . ? C9 C8 C14 120.8(4) . . ? C13 C8 C14 119.2(4) . . ? C9 C8 Ru1 70.5(2) . . ? C13 C8 Ru1 70.07(19) . . ? C14 C8 Ru1 132.2(3) . . ? C8 C9 C10 119.8(3) . . ? C8 C9 C15 120.6(4) . . ? C10 C9 C15 119.6(4) . . ? C8 C9 Ru1 72.7(2) . . ? C10 C9 Ru1 72.57(19) . . ? C15 C9 Ru1 128.9(3) . . ? C11 C10 C9 120.0(3) . . ? C11 C10 C16 120.7(4) . . ? C9 C10 C16 119.2(4) . . ? C11 C10 Ru1 72.2(2) . . ? C9 C10 Ru1 69.9(2) . . ? C16 C10 Ru1 132.8(3) . . ? C10 C11 C12 120.0(3) . . ? C10 C11 C17 120.6(4) . . ? C12 C11 C17 119.4(4) . . ? C10 C11 Ru1 71.4(2) . . ? C12 C11 Ru1 68.37(19) . . ? C17 C11 Ru1 131.7(3) . . ? C13 C12 C11 119.5(3) . . ? C13 C12 C18 120.4(4) . . ? C11 C12 C18 120.0(4) . . ? C13 C12 Ru1 72.2(2) . . ? C11 C12 Ru1 74.0(2) . . ? C18 C12 Ru1 127.2(3) . . ? C12 C13 C8 120.3(3) . . ? C12 C13 C19 120.3(4) . . ? C8 C13 C19 119.4(4) . . ? C12 C13 Ru1 70.3(2) . . ? C8 C13 Ru1 72.5(2) . . ? C19 C13 Ru1 130.7(3) . . ? F1 P1 F6 90.7(2) . . ? F1 P1 F5 90.5(2) . . ? F6 P1 F5 178.01(19) . . ? F1 P1 F3 178.88(17) . . ? F6 P1 F3 89.60(18) . . ? F5 P1 F3 89.13(17) . . ? F1 P1 F2 90.95(16) . . ? F6 P1 F2 90.47(17) . . ? F5 P1 F2 91.07(16) . . ? F3 P1 F2 90.12(15) . . ? F1 P1 F4 90.17(16) . . ? F6 P1 F4 89.57(17) . . ? F5 P1 F4 88.87(16) . . ? F3 P1 F4 88.76(15) . . ? F2 P1 F4 178.88(17) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.037 _refine_diff_density_min -1.098 _refine_diff_density_rms 0.105 #===END Complex 8 data_2163b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22H37N1S2Ru1P1F6Br1' _chemical_formula_sum 'C25.67 H41.50 Br F6 N2.83 P Ru S2' _chemical_formula_weight 779.85 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 16.7659(5) _cell_length_b 16.7659(5) _cell_length_c 45.705(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 11126.3(8) _cell_formula_units_Z 12 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3117 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 17.08 _exptl_crystal_description HEXAGONAL _exptl_crystal_colour Gold _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4744 _exptl_absorpt_coefficient_mu 1.704 _exptl_absorpt_correction_type 'Sadabs, (Shedrick 2001)' _exptl_absorpt_correction_T_min 0.5790 _exptl_absorpt_correction_T_max 0.8481 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59241 _diffrn_reflns_av_R_equivalents 0.1649 _diffrn_reflns_av_sigmaI/netI 0.0849 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 24.00 _reflns_number_total 5914 _reflns_number_gt 4378 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0945P)^2^+447.2922P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0033(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5914 _refine_ls_number_parameters 373 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.1637 _refine_ls_R_factor_gt 0.1325 _refine_ls_wR_factor_ref 0.3342 _refine_ls_wR_factor_gt 0.3183 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.570 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.30779(9) 0.31590(9) 0.62899(4) 0.0368(5) Uani 1 1 d . . . Br1 Br 0.90189(13) 0.31668(13) 0.59615(5) 0.0504(7) Uani 1 1 d . . . S1 S 0.4217(3) 0.3916(4) 0.66464(12) 0.0486(13) Uani 1 1 d . . . S2 S 0.3510(3) 0.4232(3) 0.59058(13) 0.0450(13) Uani 1 1 d . . . N1 N 0.4092(10) 0.2894(11) 0.6084(4) 0.043(4) Uani 1 1 d . . . C1 C 0.4934(15) 0.3433(16) 0.6560(6) 0.060(7) Uani 1 1 d . . . H1A H 0.5543 0.3808 0.6649 0.072 Uiso 1 1 calc R . . H1B H 0.4660 0.2808 0.6641 0.072 Uiso 1 1 calc R . . C2 C 0.5028(15) 0.3404(15) 0.6232(6) 0.064(7) Uani 1 1 d . . . H2A H 0.5380 0.3098 0.6186 0.077 Uiso 1 1 calc R . . H2B H 0.5370 0.4035 0.6156 0.077 Uiso 1 1 calc R . . C3 C 0.4352(15) 0.4062(14) 0.5707(5) 0.049(5) Uani 1 1 d . . . H3A H 0.4302 0.4141 0.5496 0.059 Uiso 1 1 calc R . . H3B H 0.4976 0.4512 0.5771 0.059 Uiso 1 1 calc R . . C4 C 0.4148(17) 0.3075(13) 0.5772(5) 0.057(6) Uani 1 1 d . . . H4A H 0.3565 0.2633 0.5680 0.069 Uiso 1 1 calc R . . H4B H 0.4636 0.2988 0.5687 0.069 Uiso 1 1 calc R . . C5 C 0.5039(13) 0.5173(13) 0.6608(5) 0.053(6) Uani 1 1 d . . . H5A H 0.5412 0.5292 0.6431 0.064 Uiso 1 1 calc R . . H5B H 0.4702 0.5509 0.6592 0.064 Uiso 1 1 calc R . . C6 C 0.564(2) 0.5478(16) 0.6872(7) 0.076(8) Uani 1 1 d . . . H6A H 0.5379 0.5474 0.7055 0.091 Uiso 1 1 calc R . . C7 C 0.648(2) 0.574(2) 0.6859(8) 0.118(14) Uani 1 1 d . . . H7A H 0.6753 0.5745 0.6678 0.141 Uiso 1 1 calc R . . H7B H 0.6844 0.5926 0.7029 0.141 Uiso 1 1 calc R . . C8 C 0.4206(14) 0.5471(12) 0.5973(5) 0.052(6) Uani 1 1 d . . . H8A H 0.3921 0.5655 0.6126 0.063 Uiso 1 1 calc R . . H8B H 0.4824 0.5628 0.6038 0.063 Uiso 1 1 calc R . . C9 C 0.4261(16) 0.5948(14) 0.5703(6) 0.063(7) Uani 1 1 d . . . H9A H 0.3718 0.5907 0.5629 0.075 Uiso 1 1 calc R . . C10 C 0.503(2) 0.6434(15) 0.5557(7) 0.085(9) Uani 1 1 d . . . H10A H 0.5579 0.6486 0.5626 0.102 Uiso 1 1 calc R . . H10B H 0.5025 0.6731 0.5382 0.102 Uiso 1 1 calc R . . C11 C 0.2161(11) 0.1710(13) 0.6433(5) 0.043(5) Uani 1 1 d U . . C12 C 0.2214(14) 0.2262(13) 0.6673(5) 0.050(5) Uani 1 1 d U . . C13 C 0.1973(14) 0.3006(13) 0.6606(5) 0.048(5) Uani 1 1 d U . . C14 C 0.1706(12) 0.3089(13) 0.6323(5) 0.048(5) Uani 1 1 d U . . C15 C 0.1645(12) 0.2496(12) 0.6089(5) 0.045(5) Uani 1 1 d U . . C16 C 0.1884(11) 0.1795(12) 0.6147(5) 0.041(5) Uani 1 1 d U . . C17 C 0.2340(15) 0.0908(13) 0.6485(5) 0.053(6) Uani 1 1 d . . . H17A H 0.1774 0.0368 0.6547 0.080 Uiso 1 1 calc R . . H17B H 0.2804 0.1078 0.6636 0.080 Uiso 1 1 calc R . . H17C H 0.2555 0.0771 0.6306 0.080 Uiso 1 1 calc R . . C18 C 0.2422(17) 0.2158(15) 0.6980(5) 0.063(7) Uani 1 1 d . . . H18A H 0.1863 0.1701 0.7076 0.095 Uiso 1 1 calc R . . H18B H 0.2663 0.2744 0.7080 0.095 Uiso 1 1 calc R . . H18C H 0.2876 0.1961 0.6985 0.095 Uiso 1 1 calc R . . C19 C 0.2068(17) 0.3641(16) 0.6854(6) 0.069(7) Uani 1 1 d . . . H19A H 0.1481 0.3402 0.6953 0.103 Uiso 1 1 calc R . . H19B H 0.2257 0.4249 0.6777 0.103 Uiso 1 1 calc R . . H19C H 0.2528 0.3680 0.6991 0.103 Uiso 1 1 calc R . . C20 C 0.1489(14) 0.3850(13) 0.6258(7) 0.073(8) Uani 1 1 d . . . H20A H 0.0839 0.3622 0.6291 0.110 Uiso 1 1 calc R . . H20B H 0.1642 0.4045 0.6056 0.110 Uiso 1 1 calc R . . H20C H 0.1849 0.4369 0.6387 0.110 Uiso 1 1 calc R . . C21 C 0.1262(14) 0.2573(16) 0.5795(7) 0.075(8) Uani 1 1 d . . . H21A H 0.0599 0.2171 0.5794 0.113 Uiso 1 1 calc R . . H21B H 0.1535 0.2394 0.5640 0.113 Uiso 1 1 calc R . . H21C H 0.1407 0.3204 0.5765 0.113 Uiso 1 1 calc R . . C22 C 0.1827(14) 0.1164(14) 0.5903(5) 0.057(6) Uani 1 1 d . . . H22A H 0.1214 0.0628 0.5898 0.086 Uiso 1 1 calc R . . H22B H 0.2276 0.0969 0.5936 0.086 Uiso 1 1 calc R . . H22C H 0.1954 0.1488 0.5718 0.086 Uiso 1 1 calc R . . P1 P 0.0000 0.0000 0.5000 0.073(5) Uani 1 6 d S . . F1 F 0.0861(12) 0.0205(12) 0.4807(4) 0.104(6) Uani 1 1 d . . . P2 P 0.2144(6) -0.0004(6) 0.7500 0.053(2) Uani 1 2 d S . . F2 F 0.1505(16) 0.0448(17) 0.7500 0.082(6) Uani 1 2 d S . . F3 F 0.283(2) -0.038(2) 0.7500 0.111(10) Uani 1 2 d S . . F4 F 0.1239(19) -0.1002(14) 0.7500 0.104(9) Uani 1 2 d S . . F5 F 0.2149(10) -0.0010(9) 0.7154(3) 0.070(4) Uani 1 1 d . . . F6 F 0.3000(17) 0.0980(17) 0.7500 0.113(9) Uani 1 2 d S . . P3 P 0.3333 0.6667 0.6681(2) 0.042(2) Uani 1 3 d S . . F7 F 0.385(3) 0.638(2) 0.6874(9) 0.28(2) Uani 1 1 d . . . F8 F 0.2950(17) 0.5781(12) 0.6503(7) 0.168(11) Uani 1 1 d . . . N1S N 0.0000 0.0000 0.6447(9) 0.065(9) Uani 1 3 d SU . . C1S C 0.0000 0.0000 0.6977(10) 0.061(11) Uani 1 3 d SU . . H1S1 H -0.0630 -0.0302 0.7048 0.092 Uiso 0.33 1 calc PR . . H1S2 H 0.0328 0.0630 0.7048 0.092 Uiso 0.33 1 calc PR . . H1S3 H 0.0302 -0.0328 0.7048 0.092 Uiso 0.33 1 calc PR . . C2S C 0.0000 0.0000 0.6685(9) 0.027(7) Uani 1 3 d SU . . N2S N 0.388(4) 0.475(5) 0.7500 0.16(2) Uani 1 2 d S . . C3S C 0.254(4) 0.503(3) 0.7500 0.112(18) Uani 1 2 d S . . H3S1 H 0.2157 0.4746 0.7330 0.169 Uiso 0.50 1 calc PR . . H3S2 H 0.2794 0.5688 0.7494 0.169 Uiso 1 2 calc SR . . H3S3 H 0.2179 0.4779 0.7676 0.169 Uiso 0.50 1 calc PR . . C4S C 0.331(4) 0.482(3) 0.7500 0.100(15) Uani 1 2 d S . . N3S N 0.290(3) -0.027(5) 0.4873(11) 0.24(3) Uani 1 1 d . . . C5S C 0.263(2) 0.053(4) 0.5247(8) 0.140(18) Uani 1 1 d . . . H5SA H 0.3030 0.0705 0.5416 0.210 Uiso 1 1 calc R . . H5SB H 0.1995 0.0129 0.5309 0.210 Uiso 1 1 calc R . . H5SC H 0.2682 0.1074 0.5155 0.210 Uiso 1 1 calc R . . C6S C 0.286(4) 0.008(3) 0.5057(10) 0.15(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 0.0217(8) 0.0211(8) 0.0631(11) -0.0003(7) 0.0032(7) 0.0071(6) Br1 0.0370(11) 0.0273(10) 0.0836(16) -0.0001(10) -0.0019(10) 0.0137(8) S1 0.036(3) 0.037(3) 0.061(3) -0.001(2) 0.000(2) 0.009(2) S2 0.033(2) 0.025(2) 0.076(4) 0.008(2) 0.002(2) 0.013(2) N1 0.030(8) 0.036(9) 0.062(12) -0.003(8) 0.005(8) 0.016(7) C1 0.047(13) 0.049(13) 0.10(2) -0.013(13) -0.029(13) 0.038(11) C2 0.042(12) 0.033(11) 0.11(2) -0.014(13) -0.015(13) 0.016(10) C3 0.053(13) 0.037(11) 0.055(13) 0.004(10) 0.016(10) 0.021(10) C4 0.072(15) 0.028(10) 0.077(17) -0.007(11) 0.015(13) 0.028(11) C5 0.022(9) 0.030(11) 0.094(18) -0.009(11) -0.003(10) 0.003(8) C6 0.073(19) 0.038(13) 0.10(2) -0.008(13) -0.017(16) 0.012(13) C7 0.06(2) 0.12(3) 0.11(3) -0.02(2) -0.006(18) -0.001(19) C8 0.040(11) 0.024(10) 0.077(16) 0.000(10) 0.013(11) 0.004(9) C9 0.046(13) 0.036(12) 0.102(19) 0.023(13) 0.006(13) 0.017(11) C10 0.10(2) 0.028(12) 0.11(2) 0.016(13) -0.001(18) 0.013(13) C11 0.009(7) 0.033(9) 0.076(13) -0.008(9) 0.009(8) 0.003(7) C12 0.037(10) 0.027(9) 0.081(14) 0.011(10) 0.014(10) 0.013(8) C13 0.040(10) 0.029(9) 0.078(14) -0.007(9) 0.010(10) 0.020(8) C14 0.020 0.036(10) 0.090(14) -0.008(10) 0.001(9) 0.016(6) C15 0.018(8) 0.022(9) 0.085(14) -0.003(9) -0.011(9) 0.002(7) C16 0.008(7) 0.028(9) 0.078(13) 0.005(9) -0.002(8) 0.003(7) C17 0.055(13) 0.033(11) 0.077(16) 0.008(10) 0.025(12) 0.025(10) C18 0.069(16) 0.045(13) 0.079(18) 0.024(12) 0.023(13) 0.032(12) C19 0.061(15) 0.048(13) 0.10(2) -0.010(13) 0.021(14) 0.028(12) C20 0.036(11) 0.029(10) 0.17(3) -0.011(14) -0.013(14) 0.026(9) C21 0.025(11) 0.044(13) 0.14(3) 0.006(15) -0.007(14) 0.008(10) C22 0.043(12) 0.042(12) 0.083(17) -0.032(12) -0.015(11) 0.019(10) P1 0.065(7) 0.065(7) 0.089(13) 0.000 0.000 0.033(3) F1 0.084(11) 0.086(12) 0.135(15) -0.003(11) 0.023(11) 0.036(10) P2 0.052(5) 0.046(5) 0.067(6) 0.000 0.000 0.029(4) F2 0.089(15) 0.110(18) 0.074(14) 0.000 0.000 0.070(15) F3 0.17(3) 0.18(3) 0.086(16) 0.000 0.000 0.16(2) F4 0.13(2) 0.050(12) 0.071(15) 0.000 0.000 0.003(13) F5 0.091(10) 0.052(8) 0.076(9) 0.012(7) 0.018(8) 0.043(8) F6 0.082(17) 0.075(16) 0.12(2) 0.000 0.000 -0.005(13) P3 0.029(3) 0.029(3) 0.068(6) 0.000 0.000 0.0146(13) F7 0.26(4) 0.13(2) 0.36(4) 0.04(3) -0.22(4) 0.04(2) F8 0.15(2) 0.048(10) 0.28(3) -0.047(15) 0.00(2) 0.031(12) N1S 0.064(14) 0.064(14) 0.07(2) 0.000 0.000 0.032(7) C1S 0.044(13) 0.044(13) 0.10(3) 0.000 0.000 0.022(7) C2S 0.007(8) 0.007(8) 0.07(2) 0.000 0.000 0.003(4) N2S 0.10(4) 0.25(7) 0.15(5) 0.000 0.000 0.11(5) C3S 0.13(5) 0.06(3) 0.12(4) 0.000 0.000 0.03(3) C4S 0.07(3) 0.07(3) 0.12(4) 0.000 0.000 0.00(2) N3S 0.11(3) 0.40(9) 0.18(4) -0.11(5) -0.02(3) 0.11(4) C5S 0.06(2) 0.25(6) 0.09(3) 0.02(3) -0.003(18) 0.07(3) C6S 0.18(5) 0.16(4) 0.10(3) -0.05(3) 0.04(3) 0.08(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.174(15) . ? Ru1 C11 2.227(19) . ? Ru1 C14 2.249(17) . ? Ru1 C16 2.255(18) . ? Ru1 C13 2.26(2) . ? Ru1 C15 2.275(18) . ? Ru1 C12 2.29(2) . ? Ru1 S1 2.343(6) . ? Ru1 S2 2.353(5) . ? S1 C1 1.80(2) . ? S1 C5 1.862(19) . ? S2 C3 1.82(2) . ? S2 C8 1.829(19) . ? N1 C4 1.45(3) . ? N1 C2 1.52(3) . ? C1 C2 1.51(3) . ? C3 C4 1.54(3) . ? C5 C6 1.49(3) . ? C6 C7 1.26(4) . ? C8 C9 1.45(3) . ? C9 C10 1.31(4) . ? C11 C12 1.41(3) . ? C11 C16 1.42(3) . ? C11 C17 1.54(3) . ? C12 C18 1.48(3) . ? C12 C13 1.52(3) . ? C13 C14 1.40(3) . ? C13 C19 1.51(3) . ? C14 C15 1.43(3) . ? C14 C20 1.52(3) . ? C15 C16 1.44(3) . ? C15 C21 1.52(3) . ? C16 C22 1.51(3) . ? P1 F1 1.576(17) 3 ? P1 F1 1.576(17) 9_556 ? P1 F1 1.576(17) 8_556 ? P1 F1 1.576(17) . ? P1 F1 1.576(17) 7_556 ? P1 F1 1.576(17) 2 ? P2 F6 1.55(2) . ? P2 F3 1.57(2) . ? P2 F5 1.581(14) 10_557 ? P2 F5 1.581(14) . ? P2 F2 1.59(2) . ? P2 F4 1.60(2) . ? P3 F7 1.47(2) 2_665 ? P3 F7 1.47(3) 3_565 ? P3 F7 1.47(2) . ? P3 F8 1.53(2) 3_565 ? P3 F8 1.53(2) . ? P3 F8 1.53(2) 2_665 ? N1S C2S 1.09(4) . ? C1S C2S 1.34(5) . ? N2S C4S 1.04(7) . ? C3S C4S 1.48(7) . ? N3S C6S 1.05(5) . ? C5S C6S 1.33(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 N1 Ru1 C11 95.0(6) . . ? N1 Ru1 C14 154.4(7) . . ? C11 Ru1 C14 78.1(7) . . ? N1 Ru1 C16 93.2(6) . . ? C11 Ru1 C16 36.8(7) . . ? C14 Ru1 C16 66.4(7) . . ? N1 Ru1 C13 159.0(7) . . ? C11 Ru1 C13 67.0(7) . . ? C14 Ru1 C13 36.1(8) . . ? C16 Ru1 C13 78.9(7) . . ? N1 Ru1 C15 117.9(7) . . ? C11 Ru1 C15 66.5(7) . . ? C14 Ru1 C15 36.8(8) . . ? C16 Ru1 C15 37.1(6) . . ? C13 Ru1 C15 66.2(8) . . ? N1 Ru1 C12 119.9(7) . . ? C11 Ru1 C12 36.3(7) . . ? C14 Ru1 C12 67.7(8) . . ? C16 Ru1 C12 66.8(8) . . ? C13 Ru1 C12 39.1(7) . . ? C15 Ru1 C12 79.6(8) . . ? N1 Ru1 S1 84.4(5) . . ? C11 Ru1 S1 108.5(6) . . ? C14 Ru1 S1 121.2(6) . . ? C16 Ru1 S1 145.1(5) . . ? C13 Ru1 S1 91.0(6) . . ? C15 Ru1 S1 157.0(6) . . ? C12 Ru1 S1 84.3(6) . . ? N1 Ru1 S2 82.0(5) . . ? C11 Ru1 S2 146.5(6) . . ? C14 Ru1 S2 90.3(6) . . ? C16 Ru1 S2 109.7(6) . . ? C13 Ru1 S2 119.0(6) . . ? C15 Ru1 S2 85.4(5) . . ? C12 Ru1 S2 157.5(5) . . ? S1 Ru1 S2 104.39(19) . . ? C1 S1 C5 101.9(11) . . ? C1 S1 Ru1 98.7(8) . . ? C5 S1 Ru1 119.2(8) . . ? C3 S2 C8 99.1(10) . . ? C3 S2 Ru1 102.7(7) . . ? C8 S2 Ru1 121.4(8) . . ? C4 N1 C2 112.3(18) . . ? C4 N1 Ru1 111.0(13) . . ? C2 N1 Ru1 112.6(13) . . ? C2 C1 S1 109.6(15) . . ? C1 C2 N1 111.4(19) . . ? C4 C3 S2 107.4(14) . . ? N1 C4 C3 111.8(17) . . ? C6 C5 S1 107.5(16) . . ? C7 C6 C5 122(3) . . ? C9 C8 S2 108.2(16) . . ? C10 C9 C8 123(2) . . ? C12 C11 C16 124.5(18) . . ? C12 C11 C17 119(2) . . ? C16 C11 C17 116.7(18) . . ? C12 C11 Ru1 74.3(11) . . ? C16 C11 Ru1 72.7(11) . . ? C17 C11 Ru1 132.1(12) . . ? C11 C12 C18 127.1(19) . . ? C11 C12 C13 115(2) . . ? C18 C12 C13 117.6(19) . . ? C11 C12 Ru1 69.4(12) . . ? C18 C12 Ru1 134.0(15) . . ? C13 C12 Ru1 69.4(11) . . ? C14 C13 C19 123.5(19) . . ? C14 C13 C12 119.8(18) . . ? C19 C13 C12 117(2) . . ? C14 C13 Ru1 71.5(11) . . ? C19 C13 Ru1 127.5(15) . . ? C12 C13 Ru1 71.5(11) . . ? C13 C14 C15 122.5(18) . . ? C13 C14 C20 119(2) . . ? C15 C14 C20 118(2) . . ? C13 C14 Ru1 72.4(11) . . ? C15 C14 Ru1 72.6(10) . . ? C20 C14 Ru1 127.6(14) . . ? C14 C15 C16 119(2) . . ? C14 C15 C21 119.1(18) . . ? C16 C15 C21 122(2) . . ? C14 C15 Ru1 70.6(10) . . ? C16 C15 Ru1 70.7(10) . . ? C21 C15 Ru1 134.6(14) . . ? C11 C16 C15 119.3(19) . . ? C11 C16 C22 121.4(17) . . ? C15 C16 C22 119.3(19) . . ? C11 C16 Ru1 70.5(10) . . ? C15 C16 Ru1 72.2(10) . . ? C22 C16 Ru1 129.7(13) . . ? F1 P1 F1 180.0(12) 3 9_556 ? F1 P1 F1 88.2(10) 3 8_556 ? F1 P1 F1 91.8(10) 9_556 8_556 ? F1 P1 F1 91.8(10) 3 . ? F1 P1 F1 88.2(10) 9_556 . ? F1 P1 F1 88.2(10) 8_556 . ? F1 P1 F1 88.2(10) 3 7_556 ? F1 P1 F1 91.8(10) 9_556 7_556 ? F1 P1 F1 91.8(10) 8_556 7_556 ? F1 P1 F1 180.0(14) . 7_556 ? F1 P1 F1 91.8(10) 3 2 ? F1 P1 F1 88.2(10) 9_556 2 ? F1 P1 F1 180.0(12) 8_556 2 ? F1 P1 F1 91.8(10) . 2 ? F1 P1 F1 88.2(10) 7_556 2 ? F6 P2 F3 87.3(18) . . ? F6 P2 F5 90.1(6) . 10_557 ? F3 P2 F5 89.5(6) . 10_557 ? F6 P2 F5 90.1(6) . . ? F3 P2 F5 89.5(6) . . ? F5 P2 F5 178.9(12) 10_557 . ? F6 P2 F2 88.8(15) . . ? F3 P2 F2 176.0(17) . . ? F5 P2 F2 90.6(6) 10_557 . ? F5 P2 F2 90.6(6) . . ? F6 P2 F4 177.9(18) . . ? F3 P2 F4 94.8(17) . . ? F5 P2 F4 89.9(6) 10_557 . ? F5 P2 F4 89.9(6) . . ? F2 P2 F4 89.2(16) . . ? F7 P3 F7 88(3) 2_665 3_565 ? F7 P3 F7 88(3) 2_665 . ? F7 P3 F7 88(3) 3_565 . ? F7 P3 F8 86(2) 2_665 3_565 ? F7 P3 F8 91.8(17) 3_565 3_565 ? F7 P3 F8 174.1(19) . 3_565 ? F7 P3 F8 174.1(19) 2_665 . ? F7 P3 F8 86(2) 3_565 . ? F7 P3 F8 91.8(17) . . ? F8 P3 F8 94.1(16) 3_565 . ? F7 P3 F8 91.8(17) 2_665 2_665 ? F7 P3 F8 174.1(19) 3_565 2_665 ? F7 P3 F8 86(2) . 2_665 ? F8 P3 F8 94.1(16) 3_565 2_665 ? F8 P3 F8 94.1(16) . 2_665 ? N1S C2S C1S 180.00(2) . . ? N2S C4S C3S 175(6) . . ? N3S C6S C5S 164(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.360 _refine_diff_density_min -1.613 _refine_diff_density_rms 0.210 #===END Complex 9 data_3066 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H34 F6 N P Ru S2' _chemical_formula_weight 598.64 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.9741(5) _cell_length_b 16.8112(9) _cell_length_c 15.8708(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.5870(10) _cell_angle_gamma 90.00 _cell_volume 2391.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4093 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.64 _exptl_crystal_description Multifaceted _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.952 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.8324 _exptl_absorpt_correction_T_max 0.8943 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16640 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5492 _reflns_number_gt 4470 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0454P)^2^+1.5940P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5492 _refine_ls_number_parameters 314 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1000 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.046 _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 0.49409(2) 0.602356(13) 0.248910(14) 0.02177(9) Uani 1 1 d . A . S1 S 0.45051(10) 0.48639(5) 0.32996(6) 0.0381(2) Uani 1 1 d D . . S2 S 0.72821(9) 0.62670(6) 0.31390(5) 0.03440(19) Uani 1 1 d D . . N1 N 0.4164(3) 0.66069(17) 0.35964(17) 0.0298(6) Uani 1 1 d D . . H1 H 0.341(4) 0.686(2) 0.341(2) 0.034(10) Uiso 1 1 d . . . C1 C 0.3108(5) 0.5338(3) 0.3952(3) 0.0444(11) Uani 0.85 1 d PD A 1 H1A H 0.2195 0.5444 0.3608 0.053 Uiso 0.85 1 calc PR A 1 H1B H 0.2858 0.4981 0.4413 0.053 Uiso 0.85 1 calc PR A 1 C2 C 0.3730(5) 0.6105(2) 0.4305(3) 0.0414(10) Uani 0.85 1 d PD A 1 H2A H 0.2976 0.6377 0.4628 0.050 Uiso 0.85 1 calc PR A 1 H2B H 0.4600 0.5997 0.4684 0.050 Uiso 0.85 1 calc PR A 1 C1X C 0.374(3) 0.5228(11) 0.4241(12) 0.040(6) Uiso 0.15 1 d PD A 2 H1XA H 0.2984 0.4865 0.4443 0.048 Uiso 0.15 1 calc PR A 2 H1XB H 0.4525 0.5300 0.4687 0.048 Uiso 0.15 1 calc PR A 2 C2X C 0.3055(14) 0.6029(9) 0.3971(9) 0.028(5) Uiso 0.15 1 d PD A 2 H2XA H 0.2240 0.5931 0.3552 0.033 Uiso 0.15 1 calc PR A 2 H2XB H 0.2627 0.6279 0.4462 0.033 Uiso 0.15 1 calc PR A 2 C3 C 0.5312(5) 0.7220(3) 0.3908(3) 0.0436(10) Uani 0.85 1 d PD A 1 H3A H 0.5386 0.7642 0.3486 0.052 Uiso 0.85 1 calc PR A 1 H3B H 0.4987 0.7462 0.4431 0.052 Uiso 0.85 1 calc PR A 1 C4 C 0.6822(5) 0.6839(4) 0.4067(4) 0.0556(14) Uani 0.85 1 d PD A 1 H4A H 0.6803 0.6489 0.4560 0.067 Uiso 0.85 1 calc PR A 1 H4B H 0.7578 0.7251 0.4181 0.067 Uiso 0.85 1 calc PR A 1 C3X C 0.523(2) 0.6766(16) 0.4310(10) 0.040(5) Uiso 0.15 1 d PD A 2 H3XA H 0.5450 0.6282 0.4638 0.049 Uiso 0.15 1 calc PR A 2 H3XB H 0.4860 0.7177 0.4684 0.049 Uiso 0.15 1 calc PR A 2 C4X C 0.661(3) 0.7054(11) 0.3860(11) 0.043(10) Uiso 0.15 1 d PD A 2 H4XA H 0.7410 0.7187 0.4279 0.051 Uiso 0.15 1 calc PR A 2 H4XB H 0.6364 0.7535 0.3535 0.051 Uiso 0.15 1 calc PR A 2 C5 C 0.8160(4) 0.5428(3) 0.3700(2) 0.0515(11) Uani 1 1 d . A . H5A H 0.9016 0.5618 0.4048 0.062 Uiso 1 1 calc R . . H5B H 0.7445 0.5189 0.4074 0.062 Uiso 1 1 calc R . . C6 C 0.8675(5) 0.4807(2) 0.3093(3) 0.0551(11) Uani 1 1 d D . . H6A H 0.7782 0.4601 0.2788 0.066 Uiso 1 1 calc R A 1 H6B H 0.9263 0.5083 0.2677 0.066 Uiso 1 1 calc R A 1 C7 C 0.9570(6) 0.4102(3) 0.3396(4) 0.0426(12) Uani 0.70 1 d P A 1 H7A H 0.9960 0.3754 0.2998 0.051 Uiso 0.70 1 calc PR A 1 C8 C 0.9819(7) 0.3960(4) 0.4193(4) 0.0473(13) Uani 0.70 1 d P A 1 H8A H 0.9435 0.4304 0.4597 0.057 Uiso 0.70 1 calc PR A 1 H8B H 1.0384 0.3514 0.4366 0.057 Uiso 0.70 1 calc PR A 1 C7X C 0.9213(16) 0.4229(7) 0.3818(8) 0.043(3) Uiso 0.30 1 d PD A 2 H7XA H 0.8639 0.4180 0.4297 0.052 Uiso 0.30 1 calc PR A 2 C8X C 1.0379(18) 0.3831(9) 0.3780(11) 0.055(4) Uiso 0.30 1 d P A 2 H8XA H 1.0964 0.3873 0.3305 0.066 Uiso 0.30 1 calc PR A 2 H8XB H 1.0674 0.3489 0.4225 0.066 Uiso 0.30 1 calc PR A 2 C9 C 0.4146(3) 0.69891(18) 0.16058(19) 0.0279(6) Uani 1 1 d . . . C10 C 0.2992(3) 0.63935(19) 0.16502(19) 0.0287(7) Uani 1 1 d . A . C11 C 0.3303(4) 0.5594(2) 0.14678(19) 0.0313(7) Uani 1 1 d . . . C12 C 0.4796(4) 0.53580(19) 0.12900(19) 0.0304(7) Uani 1 1 d . A . C13 C 0.5931(3) 0.59413(19) 0.12356(19) 0.0294(7) Uani 1 1 d . . . C14 C 0.5596(4) 0.6765(2) 0.13792(19) 0.0301(7) Uani 1 1 d . A . C15 C 0.3782(4) 0.7849(2) 0.1759(2) 0.0443(9) Uani 1 1 d . A . H15A H 0.4695 0.8140 0.1894 0.066 Uiso 1 1 calc R . . H15B H 0.3124 0.7888 0.2225 0.066 Uiso 1 1 calc R . . H15C H 0.3293 0.8072 0.1255 0.066 Uiso 1 1 calc R . . C16 C 0.1442(4) 0.6642(2) 0.1875(2) 0.0419(9) Uani 1 1 d . . . H16A H 0.0848 0.6755 0.1363 0.063 Uiso 1 1 calc R A . H16B H 0.1503 0.7116 0.2224 0.063 Uiso 1 1 calc R . . H16C H 0.0980 0.6216 0.2182 0.063 Uiso 1 1 calc R . . C17 C 0.2082(4) 0.4980(2) 0.1479(2) 0.0464(9) Uani 1 1 d . A . H17A H 0.2153 0.4692 0.2009 0.070 Uiso 1 1 calc R . . H17B H 0.2188 0.4611 0.1016 0.070 Uiso 1 1 calc R . . H17C H 0.1120 0.5242 0.1420 0.070 Uiso 1 1 calc R . . C18 C 0.5131(5) 0.4486(2) 0.1144(2) 0.0463(9) Uani 1 1 d . . . H18A H 0.4857 0.4348 0.0564 0.069 Uiso 1 1 calc R A . H18B H 0.4562 0.4163 0.1521 0.069 Uiso 1 1 calc R . . H18C H 0.6187 0.4390 0.1253 0.069 Uiso 1 1 calc R . . C19 C 0.7493(4) 0.5717(3) 0.1008(2) 0.0440(9) Uani 1 1 d . A . H19A H 0.7605 0.5144 0.1033 0.066 Uiso 1 1 calc R . . H19B H 0.8208 0.5964 0.1403 0.066 Uiso 1 1 calc R . . H19C H 0.7668 0.5901 0.0441 0.066 Uiso 1 1 calc R . . C20 C 0.6805(4) 0.7384(2) 0.1298(2) 0.0444(9) Uani 1 1 d . . . H20A H 0.6378 0.7911 0.1349 0.067 Uiso 1 1 calc R A . H20B H 0.7242 0.7332 0.0753 0.067 Uiso 1 1 calc R . . H20C H 0.7572 0.7307 0.1741 0.067 Uiso 1 1 calc R . . P1 P 0.08134(10) 0.80610(5) 0.42102(6) 0.0363(2) Uani 1 1 d . . . F1 F 0.2050(3) 0.81370(19) 0.35200(19) 0.0851(9) Uani 1 1 d . . . F2 F 0.0665(3) 0.71463(14) 0.39606(16) 0.0617(7) Uani 1 1 d . . . F3 F -0.0385(3) 0.79427(17) 0.49001(16) 0.0683(7) Uani 1 1 d . . . F4 F 0.0967(4) 0.89571(14) 0.4466(3) 0.0941(11) Uani 1 1 d . . . F5 F 0.2120(3) 0.78471(18) 0.48758(17) 0.0751(8) Uani 1 1 d . . . F6 F -0.0496(3) 0.82368(19) 0.35353(18) 0.0814(9) 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 0.02182(13) 0.02195(13) 0.02154(13) 0.00047(9) 0.00112(9) 0.00022(9) S1 0.0479(5) 0.0265(4) 0.0403(5) 0.0086(4) 0.0050(4) -0.0004(4) S2 0.0258(4) 0.0475(5) 0.0297(4) -0.0044(4) -0.0005(3) -0.0021(4) N1 0.0304(14) 0.0342(15) 0.0247(14) -0.0018(11) -0.0002(11) 0.0084(12) C1 0.045(3) 0.055(3) 0.034(2) 0.008(2) 0.014(2) -0.009(2) C2 0.048(3) 0.045(3) 0.032(2) 0.0019(18) 0.011(2) 0.008(2) C3 0.048(3) 0.042(2) 0.041(2) -0.022(2) -0.001(2) -0.002(2) C4 0.040(3) 0.077(4) 0.049(3) -0.033(3) 0.000(2) -0.008(3) C5 0.036(2) 0.082(3) 0.035(2) 0.017(2) -0.0100(16) -0.003(2) C6 0.044(2) 0.054(2) 0.067(3) 0.016(2) 0.000(2) 0.0065(19) C7 0.040(3) 0.046(3) 0.042(3) -0.004(2) -0.003(3) 0.007(2) C8 0.048(3) 0.052(3) 0.042(3) 0.010(3) -0.001(3) 0.003(3) C9 0.0324(16) 0.0277(15) 0.0235(15) 0.0062(12) -0.0009(12) 0.0000(13) C10 0.0249(15) 0.0389(18) 0.0222(15) 0.0048(13) 0.0000(12) 0.0023(13) C11 0.0321(16) 0.0382(18) 0.0233(15) 0.0008(13) -0.0029(13) -0.0082(14) C12 0.0374(17) 0.0317(17) 0.0221(15) -0.0059(12) 0.0004(13) 0.0000(14) C13 0.0285(16) 0.0373(18) 0.0225(15) -0.0001(13) 0.0029(12) 0.0023(13) C14 0.0322(16) 0.0335(17) 0.0244(15) 0.0075(13) -0.0009(13) -0.0021(14) C15 0.050(2) 0.0312(18) 0.052(2) 0.0058(16) 0.0062(18) 0.0071(16) C16 0.0273(17) 0.057(2) 0.041(2) 0.0068(17) -0.0004(15) 0.0064(16) C17 0.042(2) 0.047(2) 0.050(2) -0.0108(18) 0.0000(17) -0.0183(17) C18 0.058(2) 0.0330(19) 0.048(2) -0.0109(16) 0.0014(18) 0.0054(17) C19 0.0322(18) 0.062(2) 0.039(2) -0.0013(18) 0.0106(15) 0.0066(17) C20 0.042(2) 0.047(2) 0.044(2) 0.0125(17) 0.0079(17) -0.0115(17) P1 0.0352(5) 0.0357(5) 0.0388(5) -0.0015(4) 0.0102(4) 0.0008(4) F1 0.0785(19) 0.102(2) 0.079(2) -0.0045(17) 0.0449(16) -0.0190(17) F2 0.0661(15) 0.0475(13) 0.0713(17) -0.0199(12) -0.0016(13) 0.0018(12) F3 0.0582(15) 0.093(2) 0.0561(15) -0.0185(14) 0.0276(12) -0.0204(14) F4 0.094(2) 0.0373(15) 0.154(3) -0.0186(16) 0.037(2) -0.0124(14) F5 0.0555(15) 0.101(2) 0.0675(17) -0.0282(15) -0.0172(13) 0.0163(14) F6 0.0791(19) 0.091(2) 0.0728(19) 0.0227(16) -0.0141(15) 0.0260(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.156(3) . ? Ru1 C12 2.206(3) . ? Ru1 C13 2.219(3) . ? Ru1 C10 2.238(3) . ? Ru1 C9 2.240(3) . ? Ru1 C11 2.257(3) . ? Ru1 C14 2.258(3) . ? Ru1 S2 2.3345(8) . ? Ru1 S1 2.3777(8) . ? S1 C1X 1.780(16) . ? S1 C1 1.843(4) . ? S2 C4 1.822(5) . ? S2 C5 1.828(4) . ? S2 C4X 1.865(18) . ? N1 C2 1.473(5) . ? N1 C3X 1.475(10) . ? N1 C3 1.524(5) . ? N1 C2X 1.530(9) . ? C1 C2 1.503(5) . ? C1X C2X 1.535(10) . ? C3 C4 1.509(6) . ? C3X C4X 1.536(10) . ? C5 C6 1.507(6) . ? C6 C7 1.499(7) . ? C6 C7X 1.567(9) . ? C7 C8 1.296(8) . ? C7X C8X 1.25(2) . ? C9 C14 1.417(4) . ? C9 C10 1.445(4) . ? C9 C15 1.504(5) . ? C10 C11 1.405(5) . ? C10 C16 1.510(4) . ? C11 C12 1.438(4) . ? C11 C17 1.506(4) . ? C12 C13 1.419(4) . ? C12 C18 1.516(5) . ? C13 C14 1.437(5) . ? C13 C19 1.511(4) . ? C14 C20 1.513(5) . ? P1 F4 1.564(3) . ? P1 F6 1.581(3) . ? P1 F3 1.582(2) . ? P1 F5 1.584(3) . ? P1 F2 1.592(2) . ? P1 F1 1.599(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 N1 Ru1 C12 157.70(12) . . ? N1 Ru1 C13 156.41(11) . . ? C12 Ru1 C13 37.41(12) . . ? N1 Ru1 C10 94.92(11) . . ? C12 Ru1 C10 67.27(12) . . ? C13 Ru1 C10 79.50(11) . . ? N1 Ru1 C9 94.30(11) . . ? C12 Ru1 C9 79.80(12) . . ? C13 Ru1 C9 67.24(11) . . ? C10 Ru1 C9 37.65(11) . . ? N1 Ru1 C11 120.45(11) . . ? C12 Ru1 C11 37.56(12) . . ? C13 Ru1 C11 67.07(11) . . ? C10 Ru1 C11 36.43(12) . . ? C9 Ru1 C11 66.66(11) . . ? N1 Ru1 C14 119.36(12) . . ? C12 Ru1 C14 67.31(12) . . ? C13 Ru1 C14 37.44(12) . . ? C10 Ru1 C14 66.83(11) . . ? C9 Ru1 C14 36.72(11) . . ? C11 Ru1 C14 78.49(11) . . ? N1 Ru1 S2 82.98(8) . . ? C12 Ru1 S2 119.13(9) . . ? C13 Ru1 S2 91.05(8) . . ? C10 Ru1 S2 151.37(9) . . ? C9 Ru1 S2 113.83(8) . . ? C11 Ru1 S2 156.54(9) . . ? C14 Ru1 S2 89.25(8) . . ? N1 Ru1 S1 82.23(8) . . ? C12 Ru1 S1 92.64(9) . . ? C13 Ru1 S1 121.07(9) . . ? C10 Ru1 S1 113.98(9) . . ? C9 Ru1 S1 151.30(8) . . ? C11 Ru1 S1 90.49(8) . . ? C14 Ru1 S1 158.41(9) . . ? S2 Ru1 S1 94.10(3) . . ? C1X S1 C1 23.5(7) . . ? C1X S1 Ru1 104.5(6) . . ? C1 S1 Ru1 94.70(15) . . ? C4 S2 C5 97.0(3) . . ? C4 S2 C4X 16.1(3) . . ? C5 S2 C4X 113.1(4) . . ? C4 S2 Ru1 102.56(16) . . ? C5 S2 Ru1 116.06(14) . . ? C4X S2 Ru1 95.0(8) . . ? C2 N1 C3X 72.7(10) . . ? C2 N1 C3 109.7(3) . . ? C3X N1 C3 38.9(10) . . ? C2 N1 C2X 30.7(4) . . ? C3X N1 C2X 103.2(10) . . ? C3 N1 C2X 138.2(6) . . ? C2 N1 Ru1 117.9(2) . . ? C3X N1 Ru1 119.0(9) . . ? C3 N1 Ru1 109.5(2) . . ? C2X N1 Ru1 105.5(7) . . ? C2 C1 S1 109.3(3) . . ? N1 C2 C1 108.2(3) . . ? C2X C1X S1 103.4(13) . . ? N1 C2X C1X 113.9(14) . . ? C4 C3 N1 110.9(4) . . ? C3 C4 S2 108.8(4) . . ? N1 C3X C4X 102.2(17) . . ? C3X C4X S2 110.5(16) . . ? C6 C5 S2 111.2(3) . . ? C7 C6 C5 121.2(4) . . ? C7 C6 C7X 29.6(5) . . ? C5 C6 C7X 93.1(6) . . ? C8 C7 C6 121.6(6) . . ? C8X C7X C6 121.9(14) . . ? C14 C9 C10 119.8(3) . . ? C14 C9 C15 120.4(3) . . ? C10 C9 C15 119.8(3) . . ? C14 C9 Ru1 72.31(17) . . ? C10 C9 Ru1 71.10(17) . . ? C15 C9 Ru1 131.4(2) . . ? C11 C10 C9 120.2(3) . . ? C11 C10 C16 120.5(3) . . ? C9 C10 C16 119.3(3) . . ? C11 C10 Ru1 72.53(18) . . ? C9 C10 Ru1 71.26(17) . . ? C16 C10 Ru1 129.8(2) . . ? C10 C11 C12 120.0(3) . . ? C10 C11 C17 120.1(3) . . ? C12 C11 C17 119.9(3) . . ? C10 C11 Ru1 71.04(17) . . ? C12 C11 Ru1 69.31(17) . . ? C17 C11 Ru1 131.4(2) . . ? C13 C12 C11 119.9(3) . . ? C13 C12 C18 120.7(3) . . ? C11 C12 C18 119.3(3) . . ? C13 C12 Ru1 71.79(17) . . ? C11 C12 Ru1 73.13(17) . . ? C18 C12 Ru1 128.2(2) . . ? C12 C13 C14 120.0(3) . . ? C12 C13 C19 121.2(3) . . ? C14 C13 C19 118.7(3) . . ? C12 C13 Ru1 70.81(17) . . ? C14 C13 Ru1 72.73(17) . . ? C19 C13 Ru1 130.0(2) . . ? C9 C14 C13 119.8(3) . . ? C9 C14 C20 120.6(3) . . ? C13 C14 C20 119.6(3) . . ? C9 C14 Ru1 70.97(17) . . ? C13 C14 Ru1 69.83(17) . . ? C20 C14 Ru1 131.2(2) . . ? F4 P1 F6 92.83(19) . . ? F4 P1 F3 89.80(16) . . ? F6 P1 F3 89.14(16) . . ? F4 P1 F5 89.55(18) . . ? F6 P1 F5 177.62(17) . . ? F3 P1 F5 90.91(15) . . ? F4 P1 F2 179.4(2) . . ? F6 P1 F2 87.75(15) . . ? F3 P1 F2 89.95(15) . . ? F5 P1 F2 89.87(14) . . ? F4 P1 F1 92.57(17) . . ? F6 P1 F1 92.18(17) . . ? F3 P1 F1 177.23(17) . . ? F5 P1 F1 87.67(17) . . ? F2 P1 F1 87.67(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.909 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.091 #===END Complex 10 data_2051 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H30 F6 N P Ru S2' _chemical_formula_weight 570.59 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3846(7) _cell_length_b 13.8429(7) _cell_length_c 13.7618(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.0470(10) _cell_angle_gamma 90.00 _cell_volume 2255.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7241 _cell_measurement_theta_min 2.263 _cell_measurement_theta_max 29.129 _exptl_crystal_description triclinic block _exptl_crystal_colour Red _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.6549 _exptl_absorpt_correction_T_max 0.8091 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18088 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 30.01 _reflns_number_total 6408 _reflns_number_gt 5482 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0475P)^2^+0.9280P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6408 _refine_ls_number_parameters 326 _refine_ls_number_restraints 357 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0944 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.005 _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 0.678114(15) 0.227105(13) 0.485809(13) 0.03280(7) Uani 1 1 d . . . S1 S 0.56473(6) 0.33211(6) 0.36100(6) 0.0576(2) Uani 1 1 d . . . S2 S 0.70272(7) 0.34744(5) 0.61088(5) 0.05152(17) Uani 1 1 d . . . N1 N 0.8109(2) 0.30596(18) 0.44915(18) 0.0452(5) Uani 1 1 d . . . H1 H 0.861(3) 0.272(2) 0.457(3) 0.046(9) Uiso 1 1 d . . . C1 C 0.6702(3) 0.3856(3) 0.3085(3) 0.0670(9) Uani 1 1 d . . . H1A H 0.6405 0.3880 0.2342 0.080 Uiso 1 1 calc R . . H1B H 0.6860 0.4520 0.3335 0.080 Uiso 1 1 calc R . . C2 C 0.7767(3) 0.3283(3) 0.3380(2) 0.0594(8) Uani 1 1 d . . . H2A H 0.8369 0.3649 0.3217 0.071 Uiso 1 1 calc R . . H2B H 0.7656 0.2679 0.2991 0.071 Uiso 1 1 calc R . . C3 C 0.8542(3) 0.3918(2) 0.5147(3) 0.0628(8) Uani 1 1 d . . . H3A H 0.8851 0.4384 0.4763 0.075 Uiso 1 1 calc R . . H3B H 0.9157 0.3714 0.5738 0.075 Uiso 1 1 calc R . . C4 C 0.7641(3) 0.4406(2) 0.5507(3) 0.0652(9) Uani 1 1 d . . . H4A H 0.7064 0.4691 0.4933 0.078 Uiso 1 1 calc R . . H4B H 0.7971 0.4919 0.5994 0.078 Uiso 1 1 calc R . . C5 C 0.5714(4) 0.3975(3) 0.6074(3) 0.0762(11) Uani 1 1 d . . . H5 H 0.5275 0.4273 0.5474 0.091 Uiso 1 1 calc R . . C6 C 0.5332(5) 0.3944(3) 0.6862(4) 0.0996(15) Uani 1 1 d . . . H6A H 0.5763 0.3648 0.7466 0.119 Uiso 1 1 calc R . . H6B H 0.4627 0.4217 0.6826 0.119 Uiso 1 1 calc R . . C7 C 0.7313(2) 0.08599(19) 0.4401(2) 0.0455(6) Uani 1 1 d . . . C8 C 0.7728(2) 0.09186(17) 0.54843(19) 0.0393(5) Uani 1 1 d . . . C9 C 0.6984(2) 0.11309(17) 0.60506(18) 0.0386(5) Uani 1 1 d . . . C10 C 0.5800(2) 0.12796(18) 0.5545(2) 0.0418(5) Uani 1 1 d . . . C11 C 0.5393(2) 0.12062(19) 0.4472(2) 0.0477(6) Uani 1 1 d . . . C12 C 0.6145(3) 0.0988(2) 0.3895(2) 0.0508(7) Uani 1 1 d . . . C13 C 0.8146(4) 0.0641(3) 0.3816(3) 0.0770(11) Uani 1 1 d . . . H13A H 0.7856 0.0888 0.3128 0.115 Uiso 1 1 calc R . . H13B H 0.8251 -0.0052 0.3794 0.115 Uiso 1 1 calc R . . H13C H 0.8863 0.0947 0.4149 0.115 Uiso 1 1 calc R . . C14 C 0.8960(2) 0.0717(2) 0.6006(3) 0.0607(8) Uani 1 1 d . . . H14A H 0.9099 0.0028 0.5991 0.091 Uiso 1 1 calc R . . H14B H 0.9151 0.0935 0.6705 0.091 Uiso 1 1 calc R . . H14C H 0.9420 0.1058 0.5656 0.091 Uiso 1 1 calc R . . C15 C 0.7409(3) 0.1202(3) 0.7193(2) 0.0605(8) Uani 1 1 d . . . H15A H 0.8183 0.1432 0.7395 0.091 Uiso 1 1 calc R . . H15B H 0.7378 0.0569 0.7488 0.091 Uiso 1 1 calc R . . H15C H 0.6940 0.1649 0.7432 0.091 Uiso 1 1 calc R . . C16 C 0.4988(3) 0.1483(3) 0.6143(3) 0.0655(9) Uani 1 1 d . . . H16A H 0.4470 0.0944 0.6076 0.098 Uiso 1 1 calc R . . H16B H 0.4565 0.2066 0.5887 0.098 Uiso 1 1 calc R . . H16C H 0.5404 0.1571 0.6854 0.098 Uiso 1 1 calc R . . C17 C 0.4150(3) 0.1362(3) 0.3946(3) 0.0744(11) Uani 1 1 d . . . H17A H 0.3787 0.0743 0.3742 0.112 Uiso 1 1 calc R . . H17B H 0.4061 0.1764 0.3351 0.112 Uiso 1 1 calc R . . H17C H 0.3805 0.1678 0.4409 0.112 Uiso 1 1 calc R . . C18 C 0.5694(4) 0.0916(3) 0.2749(2) 0.0853(13) Uani 1 1 d . . . H18A H 0.5288 0.1503 0.2480 0.128 Uiso 1 1 calc R . . H18B H 0.5187 0.0367 0.2568 0.128 Uiso 1 1 calc R . . H18C H 0.6318 0.0830 0.2465 0.128 Uiso 1 1 calc R . . P1 P 0.15183(8) 0.27415(7) 0.50233(8) 0.0620(2) Uani 1 1 d D . . F1 F 0.0738(6) 0.3288(9) 0.4113(6) 0.139(4) Uani 0.50 1 d PD A 1 F2 F 0.1549(10) 0.3670(6) 0.5676(8) 0.131(3) Uani 0.50 1 d PD A 1 F3 F 0.2391(6) 0.2260(9) 0.5934(7) 0.134(4) Uani 0.50 1 d PD A 1 F4 F 0.1595(9) 0.1876(7) 0.4361(10) 0.178(5) Uani 0.50 1 d PD A 1 F5 F 0.0523(6) 0.2328(7) 0.5305(9) 0.149(6) Uani 0.50 1 d PD A 1 F6 F 0.2582(6) 0.3185(6) 0.4742(6) 0.088(2) Uani 0.50 1 d PD A 1 F1A F 0.0854(8) 0.3700(5) 0.4674(12) 0.151(5) Uani 0.50 1 d PD A 2 F2A F 0.2359(9) 0.3224(11) 0.5884(8) 0.211(6) Uani 0.50 1 d PD A 2 F3A F 0.2047(8) 0.1736(6) 0.5320(11) 0.135(4) Uani 0.50 1 d PD A 2 F4A F 0.0519(9) 0.2234(9) 0.4183(7) 0.176(4) Uani 0.50 1 d PD A 2 F5A F 0.0711(8) 0.2560(8) 0.5722(8) 0.117(4) Uani 0.50 1 d PD A 2 F6A F 0.2199(9) 0.2901(8) 0.4309(9) 0.175(7) Uani 0.50 1 d PD 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 0.03313(11) 0.03364(11) 0.02883(10) 0.00238(6) 0.00470(7) 0.00189(7) S1 0.0453(4) 0.0614(4) 0.0574(4) 0.0287(4) 0.0016(3) 0.0038(3) S2 0.0681(5) 0.0400(3) 0.0472(4) -0.0049(3) 0.0181(3) 0.0039(3) N1 0.0405(12) 0.0462(12) 0.0479(13) 0.0010(10) 0.0114(10) 0.0005(10) C1 0.069(2) 0.072(2) 0.0553(18) 0.0274(16) 0.0109(15) -0.0093(17) C2 0.0637(19) 0.070(2) 0.0483(16) 0.0099(14) 0.0226(14) -0.0091(16) C3 0.0580(17) 0.0580(18) 0.070(2) -0.0102(15) 0.0149(15) -0.0200(15) C4 0.088(2) 0.0391(14) 0.074(2) -0.0097(14) 0.0325(19) -0.0146(15) C5 0.094(3) 0.0512(18) 0.097(3) 0.0062(18) 0.049(2) 0.0238(18) C6 0.128(4) 0.070(2) 0.129(4) -0.019(3) 0.081(3) 0.011(3) C7 0.0579(16) 0.0392(12) 0.0412(13) -0.0042(10) 0.0173(12) 0.0037(11) C8 0.0413(12) 0.0317(11) 0.0424(13) 0.0025(9) 0.0082(10) 0.0042(9) C9 0.0453(13) 0.0348(11) 0.0335(11) 0.0039(9) 0.0080(10) -0.0018(9) C10 0.0425(13) 0.0353(11) 0.0481(14) 0.0038(10) 0.0142(11) -0.0005(10) C11 0.0427(13) 0.0396(12) 0.0506(15) 0.0044(11) -0.0022(11) -0.0067(10) C12 0.0657(18) 0.0444(14) 0.0341(13) -0.0029(10) 0.0017(12) -0.0071(13) C13 0.107(3) 0.070(2) 0.070(2) -0.0083(18) 0.052(2) 0.018(2) C14 0.0421(15) 0.0614(18) 0.073(2) 0.0097(16) 0.0083(14) 0.0108(13) C15 0.074(2) 0.070(2) 0.0344(13) 0.0064(13) 0.0104(13) -0.0022(16) C16 0.0592(19) 0.0631(19) 0.086(2) 0.0033(17) 0.0400(18) -0.0017(15) C17 0.0426(16) 0.071(2) 0.088(3) 0.0142(19) -0.0131(16) -0.0099(15) C18 0.116(3) 0.087(3) 0.0357(16) -0.0095(16) -0.0043(18) -0.022(2) P1 0.0541(5) 0.0664(6) 0.0709(6) 0.0086(4) 0.0267(4) 0.0037(4) F1 0.096(5) 0.212(12) 0.094(5) 0.057(6) 0.005(4) 0.055(6) F2 0.165(8) 0.125(6) 0.132(7) -0.049(5) 0.087(6) 0.000(6) F3 0.072(4) 0.217(12) 0.115(6) 0.096(7) 0.031(4) 0.034(6) F4 0.129(8) 0.132(7) 0.261(14) -0.119(9) 0.039(9) -0.011(6) F5 0.047(3) 0.114(6) 0.300(17) 0.100(9) 0.073(6) 0.006(3) F6 0.070(3) 0.077(3) 0.133(7) 0.013(4) 0.056(4) -0.001(3) F1A 0.112(6) 0.071(4) 0.312(17) 0.070(7) 0.126(9) 0.027(4) F2A 0.137(9) 0.262(16) 0.191(11) -0.054(12) -0.017(9) -0.091(10) F3A 0.099(7) 0.091(5) 0.237(13) 0.060(7) 0.082(8) 0.035(5) F4A 0.196(12) 0.183(10) 0.116(7) -0.055(6) -0.006(7) -0.005(8) F5A 0.119(8) 0.148(8) 0.115(5) 0.017(4) 0.082(6) 0.013(5) F6A 0.193(12) 0.229(15) 0.168(11) 0.103(10) 0.153(11) 0.097(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.154(2) . ? Ru1 C11 2.208(3) . ? Ru1 C7 2.211(3) . ? Ru1 C12 2.217(3) . ? Ru1 C10 2.220(3) . ? Ru1 C9 2.237(2) . ? Ru1 C8 2.243(2) . ? Ru1 S2 2.3500(7) . ? Ru1 S1 2.3708(7) . ? S1 C1 1.825(3) . ? S2 C5 1.756(4) . ? S2 C4 1.815(3) . ? N1 C3 1.492(4) . ? N1 C2 1.495(4) . ? C1 C2 1.490(5) . ? C3 C4 1.507(5) . ? C5 C6 1.304(6) . ? C7 C12 1.420(4) . ? C7 C8 1.430(4) . ? C7 C13 1.513(4) . ? C8 C9 1.401(4) . ? C8 C14 1.509(4) . ? C9 C10 1.442(3) . ? C9 C15 1.508(4) . ? C10 C11 1.417(4) . ? C10 C16 1.501(4) . ? C11 C12 1.422(4) . ? C11 C17 1.512(4) . ? C12 C18 1.515(4) . ? P1 F2A 1.486(6) . ? P1 F6A 1.487(6) . ? P1 F5 1.509(5) . ? P1 F4 1.525(6) . ? P1 F1 1.538(5) . ? P1 F3A 1.542(6) . ? P1 F3 1.546(6) . ? P1 F1A 1.561(6) . ? P1 F2 1.562(6) . ? P1 F4A 1.589(7) . ? P1 F5A 1.597(6) . ? P1 F6 1.601(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 C11 151.19(11) . . ? N1 Ru1 C7 93.97(10) . . ? C11 Ru1 C7 67.51(11) . . ? N1 Ru1 C12 115.33(11) . . ? C11 Ru1 C12 37.48(12) . . ? C7 Ru1 C12 37.41(11) . . ? N1 Ru1 C10 164.62(9) . . ? C11 Ru1 C10 37.34(10) . . ? C7 Ru1 C10 79.70(10) . . ? C12 Ru1 C10 67.45(10) . . ? N1 Ru1 C9 126.88(9) . . ? C11 Ru1 C9 67.52(9) . . ? C7 Ru1 C9 66.85(9) . . ? C12 Ru1 C9 79.46(10) . . ? C10 Ru1 C9 37.75(9) . . ? N1 Ru1 C8 99.44(9) . . ? C11 Ru1 C8 79.49(9) . . ? C7 Ru1 C8 37.45(9) . . ? C12 Ru1 C8 67.36(10) . . ? C10 Ru1 C8 67.06(9) . . ? C9 Ru1 C8 36.45(9) . . ? N1 Ru1 S2 82.44(7) . . ? C11 Ru1 S2 125.05(9) . . ? C7 Ru1 S2 148.13(7) . . ? C12 Ru1 S2 162.24(9) . . ? C10 Ru1 S2 95.50(7) . . ? C9 Ru1 S2 90.01(7) . . ? C8 Ru1 S2 111.68(7) . . ? N1 Ru1 S1 81.40(7) . . ? C11 Ru1 S1 88.91(7) . . ? C7 Ru1 S1 119.87(7) . . ? C12 Ru1 S1 91.55(7) . . ? C10 Ru1 S1 113.93(7) . . ? C9 Ru1 S1 151.55(7) . . ? C8 Ru1 S1 157.23(7) . . ? S2 Ru1 S1 91.04(3) . . ? C1 S1 Ru1 101.26(11) . . ? C5 S2 C4 102.47(18) . . ? C5 S2 Ru1 109.86(15) . . ? C4 S2 Ru1 98.70(11) . . ? C3 N1 C2 113.4(3) . . ? C3 N1 Ru1 115.2(2) . . ? C2 N1 Ru1 109.71(18) . . ? C2 C1 S1 110.8(2) . . ? C1 C2 N1 110.7(3) . . ? N1 C3 C4 112.8(3) . . ? C3 C4 S2 106.3(2) . . ? C6 C5 S2 121.5(4) . . ? C12 C7 C8 120.4(3) . . ? C12 C7 C13 121.3(3) . . ? C8 C7 C13 118.3(3) . . ? C12 C7 Ru1 71.53(15) . . ? C8 C7 Ru1 72.47(14) . . ? C13 C7 Ru1 129.4(2) . . ? C9 C8 C7 119.9(2) . . ? C9 C8 C14 120.8(2) . . ? C7 C8 C14 119.3(3) . . ? C9 C8 Ru1 71.56(14) . . ? C7 C8 Ru1 70.08(14) . . ? C14 C8 Ru1 132.73(19) . . ? C8 C9 C10 120.2(2) . . ? C8 C9 C15 120.5(2) . . ? C10 C9 C15 119.2(2) . . ? C8 C9 Ru1 71.99(14) . . ? C10 C9 Ru1 70.48(14) . . ? C15 C9 Ru1 130.46(19) . . ? C11 C10 C9 119.5(2) . . ? C11 C10 C16 119.7(3) . . ? C9 C10 C16 120.8(3) . . ? C11 C10 Ru1 70.85(15) . . ? C9 C10 Ru1 71.77(14) . . ? C16 C10 Ru1 131.0(2) . . ? C10 C11 C12 120.4(2) . . ? C10 C11 C17 119.3(3) . . ? C12 C11 C17 120.3(3) . . ? C10 C11 Ru1 71.81(14) . . ? C12 C11 Ru1 71.63(15) . . ? C17 C11 Ru1 129.2(2) . . ? C7 C12 C11 119.5(2) . . ? C7 C12 C18 120.9(3) . . ? C11 C12 C18 119.6(3) . . ? C7 C12 Ru1 71.06(15) . . ? C11 C12 Ru1 70.89(15) . . ? C18 C12 Ru1 129.3(2) . . ? F2A P1 F6A 93.4(6) . . ? F2A P1 F5 113.6(7) . . ? F6A P1 F5 152.9(7) . . ? F2A P1 F4 132.7(6) . . ? F6A P1 F4 64.8(6) . . ? F5 P1 F4 93.1(5) . . ? F2A P1 F1 123.6(6) . . ? F6A P1 F1 74.4(6) . . ? F5 P1 F1 91.7(4) . . ? F4 P1 F1 91.9(5) . . ? F2A P1 F3A 92.9(5) . . ? F6A P1 F3A 91.7(5) . . ? F5 P1 F3A 84.6(5) . . ? F4 P1 F3A 49.7(5) . . ? F1 P1 F3A 140.9(6) . . ? F2A P1 F3 52.3(5) . . ? F6A P1 F3 101.7(6) . . ? F5 P1 F3 93.4(4) . . ? F4 P1 F3 89.7(5) . . ? F1 P1 F3 174.6(5) . . ? F3A P1 F3 41.7(4) . . ? F2A P1 F1A 92.6(5) . . ? F6A P1 F1A 91.2(5) . . ? F5 P1 F1A 90.2(4) . . ? F4 P1 F1A 127.1(6) . . ? F1 P1 F1A 35.2(5) . . ? F3A P1 F1A 173.6(5) . . ? F3 P1 F1A 142.8(6) . . ? F2A P1 F2 43.9(5) . . ? F6A P1 F2 109.6(6) . . ? F5 P1 F2 92.8(5) . . ? F4 P1 F2 174.1(5) . . ? F1 P1 F2 88.1(4) . . ? F3A P1 F2 130.8(5) . . ? F3 P1 F2 89.8(5) . . ? F1A P1 F2 53.1(5) . . ? F2A P1 F4A 173.2(6) . . ? F6A P1 F4A 93.2(6) . . ? F5 P1 F4A 59.9(6) . . ? F4 P1 F4A 52.3(4) . . ? F1 P1 F4A 57.0(5) . . ? F3A P1 F4A 88.5(5) . . ? F3 P1 F4A 127.6(5) . . ? F1A P1 F4A 85.6(5) . . ? F2 P1 F4A 131.7(5) . . ? F2A P1 F5A 90.4(5) . . ? F6A P1 F5A 175.9(6) . . ? F5 P1 F5A 23.5(6) . . ? F4 P1 F5A 113.3(6) . . ? F1 P1 F5A 102.3(5) . . ? F3A P1 F5A 89.5(5) . . ? F3 P1 F5A 81.8(5) . . ? F1A P1 F5A 87.2(4) . . ? F2 P1 F5A 72.4(5) . . ? F4A P1 F5A 83.0(5) . . ? F2A P1 F6 65.6(6) . . ? F6A P1 F6 28.0(6) . . ? F5 P1 F6 179.1(6) . . ? F4 P1 F6 87.6(4) . . ? F1 P1 F6 88.8(4) . . ? F3A P1 F6 95.4(5) . . ? F3 P1 F6 86.1(4) . . ? F1A P1 F6 89.8(4) . . ? F2 P1 F6 86.6(4) . . ? F4A P1 F6 121.0(5) . . ? F5A P1 F6 155.6(5) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.926 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.083 #===END Complex 11 data_2043a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18.50 H31.50 F6 N1.50 O P Ru S2' _chemical_formula_weight 601.11 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 17.947(3) _cell_length_b 21.283(4) _cell_length_c 12.559(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.396(4) _cell_angle_gamma 90.00 _cell_volume 4685.5(14) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2448 _cell_measurement_theta_min 2.418 _cell_measurement_theta_max 24.048 _exptl_crystal_description BLOCK _exptl_crystal_colour Orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 0.976 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.8674 _exptl_absorpt_correction_T_max 0.9087 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25908 _diffrn_reflns_av_R_equivalents 0.0855 _diffrn_reflns_av_sigmaI/netI 0.0952 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8258 _reflns_number_gt 5313 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0644P)^2^+5.6646P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8258 _refine_ls_number_parameters 616 _refine_ls_number_restraints 771 _refine_ls_R_factor_all 0.1236 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.1585 _refine_ls_wR_factor_gt 0.1424 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.042 _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 0.71594(4) 0.66794(3) 0.74351(5) 0.02785(19) Uani 1 1 d . . . S1 S 0.62578(15) 0.71831(11) 0.60216(18) 0.0511(7) Uani 1 1 d . . . S2 S 0.80422(15) 0.73531(11) 0.6895(2) 0.0512(7) Uani 1 1 d . . . N1 N 0.6927(4) 0.7480(3) 0.8371(6) 0.0338(17) Uani 1 1 d . . . H1 H 0.694(5) 0.739(4) 0.897(7) 0.05(3) Uiso 1 1 d . . . C1 C 0.6002(6) 0.7868(4) 0.6755(7) 0.054(3) Uani 1 1 d . . . H1A H 0.6290 0.8235 0.6595 0.065 Uiso 1 1 calc R . . H1B H 0.5458 0.7959 0.6500 0.065 Uiso 1 1 calc R . . C2 C 0.6170(5) 0.7757(4) 0.7949(7) 0.045(2) Uani 1 1 d . . . H2A H 0.6137 0.8158 0.8321 0.054 Uiso 1 1 calc R . . H2B H 0.5780 0.7477 0.8124 0.054 Uiso 1 1 calc R . . C3 C 0.7568(5) 0.7940(4) 0.8596(7) 0.046(2) Uani 1 1 d . . . H3A H 0.7978 0.7775 0.9172 0.056 Uiso 1 1 calc R . . H3B H 0.7388 0.8334 0.8859 0.056 Uiso 1 1 calc R . . C4 C 0.7878(5) 0.8073(4) 0.7601(7) 0.050(3) Uani 1 1 d . . . H4A H 0.8360 0.8304 0.7816 0.061 Uiso 1 1 calc R . . H4B H 0.7517 0.8340 0.7103 0.061 Uiso 1 1 calc R . . C5 C 0.9024(6) 0.7143(5) 0.7549(10) 0.072(3) Uani 1 1 d . . . H5A H 0.9251 0.6927 0.7005 0.086 Uiso 1 1 calc R . . H5B H 0.9310 0.7534 0.7740 0.086 Uiso 1 1 calc R . . C6 C 0.9149(6) 0.6745(5) 0.8535(12) 0.086(4) Uani 1 1 d . . . H6A H 0.8876 0.6934 0.9053 0.103 Uiso 1 1 calc R . . H6B H 0.9694 0.6752 0.8874 0.103 Uiso 1 1 calc R . . C7 C 0.8028(5) 0.5959(4) 0.8052(7) 0.038(2) Uani 1 1 d . . . C8 C 0.7651(5) 0.5809(4) 0.6945(7) 0.039(2) Uani 1 1 d . . . C9 C 0.6863(5) 0.5750(3) 0.6668(7) 0.036(2) Uani 1 1 d . . . C10 C 0.6420(5) 0.5834(4) 0.7489(7) 0.039(2) Uani 1 1 d . . . C11 C 0.6779(6) 0.6001(4) 0.8542(7) 0.040(2) Uani 1 1 d . . . C12 C 0.7597(6) 0.6052(4) 0.8847(7) 0.046(2) Uani 1 1 d . . . C13 C 0.8890(5) 0.6039(4) 0.8357(10) 0.067(3) Uani 1 1 d . . . H13A H 0.9113 0.5859 0.7778 0.080 Uiso 1 1 calc R . . H13B H 0.9090 0.5804 0.9027 0.080 Uiso 1 1 calc R . . C14 C 0.8114(6) 0.5708(5) 0.6081(9) 0.073(3) Uani 1 1 d . . . H14A H 0.8348 0.5295 0.6173 0.109 Uiso 1 1 calc R . . H14B H 0.8508 0.6026 0.6154 0.109 Uiso 1 1 calc R . . H14C H 0.7782 0.5737 0.5363 0.109 Uiso 1 1 calc R . . C15 C 0.6451(6) 0.5610(4) 0.5512(7) 0.061(3) Uani 1 1 d . . . H15A H 0.6052 0.5919 0.5279 0.092 Uiso 1 1 calc R . . H15B H 0.6227 0.5194 0.5479 0.092 Uiso 1 1 calc R . . H15C H 0.6810 0.5628 0.5035 0.092 Uiso 1 1 calc R . . C16 C 0.5562(5) 0.5779(4) 0.7159(10) 0.071(3) Uani 1 1 d . . . H16A H 0.5351 0.5752 0.7807 0.107 Uiso 1 1 calc R . . H16B H 0.5428 0.5405 0.6720 0.107 Uiso 1 1 calc R . . H16C H 0.5357 0.6146 0.6739 0.107 Uiso 1 1 calc R . . C17 C 0.6314(7) 0.6147(5) 0.9400(8) 0.083(4) Uani 1 1 d . . . H17A H 0.5794 0.6248 0.9041 0.124 Uiso 1 1 calc R . . H17B H 0.6539 0.6502 0.9838 0.124 Uiso 1 1 calc R . . H17C H 0.6314 0.5784 0.9866 0.124 Uiso 1 1 calc R . . C18 C 0.7981(7) 0.6191(5) 1.0024(8) 0.085(4) Uani 1 1 d . . . H18A H 0.7769 0.5920 1.0505 0.127 Uiso 1 1 calc R . . H18B H 0.7896 0.6626 1.0188 0.127 Uiso 1 1 calc R . . H18C H 0.8525 0.6114 1.0129 0.127 Uiso 1 1 calc R . . Ru2 Ru 0.70355(4) 0.32941(3) 0.75843(5) 0.02614(18) Uani 1 1 d . . . S3 S 0.63200(13) 0.26716(9) 0.85908(16) 0.0373(5) Uani 1 1 d . . . S4 S 0.80820(13) 0.27155(10) 0.85025(18) 0.0402(5) Uani 1 1 d . . . N2 N 0.6844(5) 0.2496(3) 0.6508(6) 0.043(2) Uani 1 1 d . . . H2 H 0.676(4) 0.258(3) 0.589(6) 0.02(2) Uiso 1 1 d . . . C19 C 0.6045(6) 0.2004(4) 0.7667(7) 0.045(2) Uani 1 1 d . . . H19A H 0.6381 0.1646 0.7917 0.054 Uiso 1 1 calc R . . H19B H 0.5520 0.1879 0.7669 0.054 Uiso 1 1 calc R . . C20 C 0.6107(5) 0.2185(4) 0.6520(7) 0.049(2) Uani 1 1 d . . . H20A H 0.6057 0.1807 0.6064 0.059 Uiso 1 1 calc R . . H20B H 0.5687 0.2469 0.6208 0.059 Uiso 1 1 calc R . . C21 C 0.7513(6) 0.2073(4) 0.6619(7) 0.055(3) Uani 1 1 d . . . H21A H 0.7879 0.2255 0.6229 0.066 Uiso 1 1 calc R . . H21B H 0.7347 0.1667 0.6281 0.066 Uiso 1 1 calc R . . C22 C 0.7896(6) 0.1971(4) 0.7778(8) 0.055(3) Uani 1 1 d . . . H22A H 0.8378 0.1748 0.7813 0.066 Uiso 1 1 calc R . . H22B H 0.7571 0.1708 0.8131 0.066 Uiso 1 1 calc R . . C23 C 0.8911(5) 0.2987(4) 0.8042(8) 0.054(3) Uani 1 1 d . . . H23A H 0.9346 0.2716 0.8341 0.065 Uiso 1 1 calc R . . H23B H 0.8814 0.2963 0.7245 0.065 Uiso 1 1 calc R . . C24 C 0.9100(5) 0.3664(4) 0.8405(9) 0.060(3) Uani 1 1 d . . . H24A H 0.9640 0.3739 0.8414 0.072 Uiso 1 1 calc R . . H24B H 0.9032 0.3710 0.9154 0.072 Uiso 1 1 calc R . . C25 C 0.7762(4) 0.4117(4) 0.7483(6) 0.0318(19) Uani 1 1 d . . . C26 C 0.7376(5) 0.4220(3) 0.8363(6) 0.035(2) Uani 1 1 d . . . C27 C 0.6582(5) 0.4160(3) 0.8189(6) 0.033(2) Uani 1 1 d . . . C28 C 0.6132(5) 0.4020(3) 0.7117(7) 0.034(2) Uani 1 1 d . . . C29 C 0.6513(5) 0.3944(3) 0.6253(6) 0.0297(19) Uani 1 1 d . . . C30 C 0.7323(5) 0.3977(3) 0.6418(6) 0.033(2) Uani 1 1 d . . . C31 C 0.8623(5) 0.4174(4) 0.7694(8) 0.054(3) Uani 1 1 d . . . H31A H 0.8766 0.4582 0.8040 0.065 Uiso 1 1 calc R . . H31B H 0.8771 0.4179 0.6987 0.065 Uiso 1 1 calc R . . C32 C 0.7817(6) 0.4407(4) 0.9477(7) 0.058(3) Uani 1 1 d . . . H32A H 0.7546 0.4738 0.9766 0.087 Uiso 1 1 calc R . . H32B H 0.8318 0.4558 0.9424 0.087 Uiso 1 1 calc R . . H32C H 0.7873 0.4046 0.9959 0.087 Uiso 1 1 calc R . . C33 C 0.6175(6) 0.4250(4) 0.9120(7) 0.058(3) Uani 1 1 d . . . H33A H 0.6536 0.4400 0.9759 0.087 Uiso 1 1 calc R . . H33B H 0.5961 0.3853 0.9285 0.087 Uiso 1 1 calc R . . H33C H 0.5769 0.4556 0.8910 0.087 Uiso 1 1 calc R . . C34 C 0.5279(5) 0.3958(4) 0.6932(8) 0.051(2) Uani 1 1 d . . . H34A H 0.5049 0.4372 0.6885 0.077 Uiso 1 1 calc R . . H34B H 0.5147 0.3729 0.7533 0.077 Uiso 1 1 calc R . . H34C H 0.5089 0.3732 0.6257 0.077 Uiso 1 1 calc R . . C35 C 0.6051(5) 0.3803(4) 0.5119(7) 0.052(2) Uani 1 1 d . . . H35A H 0.5651 0.3505 0.5167 0.079 Uiso 1 1 calc R . . H35B H 0.6382 0.3626 0.4680 0.079 Uiso 1 1 calc R . . H35C H 0.5825 0.4189 0.4784 0.079 Uiso 1 1 calc R . . C36 C 0.7690(5) 0.3868(4) 0.5459(7) 0.049(2) Uani 1 1 d . . . H36A H 0.8204 0.3711 0.5717 0.074 Uiso 1 1 calc R . . H36B H 0.7707 0.4260 0.5071 0.074 Uiso 1 1 calc R . . H36C H 0.7394 0.3562 0.4972 0.074 Uiso 1 1 calc R . . P1 P 0.99727(13) 0.85839(11) 0.97675(19) 0.0553(7) Uani 1 1 d D . . F1 F 0.9278(3) 0.9025(2) 0.9658(5) 0.164(4) Uani 1 1 d D . . F2 F 0.9808(3) 0.8513(3) 0.8511(3) 0.127(3) Uani 1 1 d D . . F3 F 1.0664(3) 0.8143(2) 0.9865(5) 0.171(5) Uani 1 1 d D . . F4 F 1.0134(3) 0.8654(3) 1.1017(3) 0.152(4) Uani 1 1 d D . . F5 F 1.0489(3) 0.9156(2) 0.9681(4) 0.113(3) Uani 1 1 d D . . F6 F 0.9453(3) 0.8014(2) 0.9843(4) 0.127(3) Uani 1 1 d D . . P2 P 0.66476(13) 0.50194(10) 0.23767(16) 0.0414(6) Uani 1 1 d D . . F7 F 0.6018(5) 0.4805(8) 0.1406(4) 0.147(15) Uani 0.40 1 d PD A 1 F8 F 0.6323(8) 0.5692(3) 0.2262(12) 0.129(12) Uani 0.40 1 d PD A 1 F9 F 0.7280(5) 0.5232(8) 0.3347(4) 0.121(13) Uani 0.40 1 d PD A 1 F10 F 0.6975(8) 0.4346(3) 0.2494(12) 0.162(17) Uani 0.40 1 d PD A 1 F7A F 0.5968(3) 0.5331(6) 0.1589(6) 0.102(5) Uani 0.60 1 d PD A 2 F8A F 0.6847(7) 0.5653(3) 0.2962(8) 0.174(13) Uani 0.60 1 d PD A 2 F9A F 0.7327(3) 0.4707(6) 0.3160(6) 0.166(11) Uani 0.60 1 d PD A 2 F10A F 0.6447(7) 0.4385(3) 0.1787(8) 0.217(16) Uani 0.60 1 d PD A 2 F11 F 0.7171(3) 0.5182(3) 0.1585(4) 0.121(3) Uani 1 1 d D A . F12 F 0.6125(3) 0.4855(3) 0.3168(3) 0.092(2) Uani 1 1 d D A . C1S C 0.9040(8) 0.4898(6) 0.2807(11) 0.099(4) Uani 1 1 d . . . H1S1 H 0.9465 0.5134 0.3227 0.148 Uiso 1 1 calc R . . H1S2 H 0.8919 0.4552 0.3242 0.148 Uiso 1 1 calc R . . H1S3 H 0.8600 0.5171 0.2605 0.148 Uiso 1 1 calc R . . N1S N 0.9251(6) 0.4647(6) 0.1801(10) 0.083(3) Uani 1 1 d . . . O1S O 0.9494(7) 0.4973(6) 0.1235(10) 0.142(4) Uani 1 1 d . . . O2S O 0.9120(6) 0.4086(5) 0.1644(8) 0.114(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0451(4) 0.0179(3) 0.0222(3) 0.0001(3) 0.0108(3) 0.0031(3) S1 0.0857(19) 0.0327(13) 0.0286(12) -0.0009(10) -0.0014(12) 0.0198(12) S2 0.0787(18) 0.0336(13) 0.0497(14) -0.0056(11) 0.0324(14) -0.0114(12) N1 0.046(5) 0.031(4) 0.025(4) -0.002(3) 0.009(4) 0.002(3) C1 0.072(7) 0.050(6) 0.040(5) 0.003(5) 0.010(5) 0.022(5) C2 0.052(6) 0.035(5) 0.050(6) 0.001(4) 0.018(5) 0.009(4) C3 0.069(7) 0.038(5) 0.035(5) -0.005(4) 0.017(5) 0.001(5) C4 0.068(7) 0.029(5) 0.056(6) -0.005(4) 0.019(5) -0.009(5) C5 0.057(7) 0.050(7) 0.118(10) -0.015(7) 0.043(7) 0.002(5) C6 0.039(6) 0.051(7) 0.158(13) -0.006(8) 0.004(7) 0.004(5) C7 0.048(5) 0.018(4) 0.046(5) 0.000(4) 0.003(5) 0.006(4) C8 0.060(6) 0.021(4) 0.037(5) -0.001(4) 0.015(5) 0.006(4) C9 0.054(6) 0.017(4) 0.031(5) -0.007(4) -0.002(4) 0.002(4) C10 0.041(5) 0.022(4) 0.048(6) 0.005(4) -0.004(5) 0.004(4) C11 0.065(6) 0.016(4) 0.043(5) 0.003(4) 0.021(5) 0.006(4) C12 0.090(8) 0.016(4) 0.027(5) 0.005(4) 0.000(5) 0.007(5) C13 0.040(6) 0.035(6) 0.116(10) -0.007(6) -0.006(6) 0.004(5) C14 0.101(9) 0.055(7) 0.082(8) -0.002(6) 0.064(7) 0.019(6) C15 0.104(8) 0.034(5) 0.036(5) -0.014(4) -0.009(6) 0.001(5) C16 0.066(7) 0.032(6) 0.115(10) 0.003(6) 0.020(7) 0.002(5) C17 0.149(12) 0.052(7) 0.072(8) 0.001(6) 0.079(9) -0.006(7) C18 0.154(12) 0.048(7) 0.034(6) 0.000(5) -0.021(7) -0.002(7) Ru2 0.0422(4) 0.0173(3) 0.0207(3) 0.0012(3) 0.0105(3) 0.0012(3) S3 0.0621(15) 0.0265(11) 0.0264(11) 0.0010(9) 0.0168(11) -0.0061(10) S4 0.0500(14) 0.0317(12) 0.0380(12) 0.0070(10) 0.0079(11) 0.0083(10) N2 0.081(6) 0.018(4) 0.034(5) 0.004(3) 0.021(5) 0.004(4) C19 0.079(7) 0.019(4) 0.040(5) -0.003(4) 0.015(5) -0.013(4) C20 0.077(7) 0.037(5) 0.035(5) -0.004(4) 0.013(5) -0.017(5) C21 0.100(8) 0.028(5) 0.042(6) -0.009(4) 0.030(6) 0.012(5) C22 0.088(8) 0.025(5) 0.056(6) 0.001(5) 0.024(6) 0.009(5) C23 0.056(6) 0.046(6) 0.061(7) 0.014(5) 0.012(5) 0.017(5) C24 0.042(6) 0.051(7) 0.085(8) 0.016(6) 0.008(6) -0.004(5) C25 0.037(5) 0.027(4) 0.029(5) 0.001(4) 0.002(4) 0.003(4) C26 0.065(6) 0.011(4) 0.026(4) -0.004(3) 0.000(4) -0.009(4) C27 0.062(6) 0.014(4) 0.024(4) 0.006(3) 0.012(4) 0.007(4) C28 0.055(6) 0.005(4) 0.043(5) 0.004(3) 0.013(5) 0.002(4) C29 0.044(5) 0.014(4) 0.027(4) 0.002(3) -0.001(4) 0.001(4) C30 0.058(6) 0.016(4) 0.027(4) 0.004(3) 0.011(4) 0.001(4) C31 0.058(6) 0.039(6) 0.062(7) 0.010(5) 0.006(5) -0.006(5) C32 0.087(8) 0.038(6) 0.038(5) -0.011(5) -0.011(5) -0.004(5) C33 0.095(8) 0.041(6) 0.047(6) -0.003(5) 0.035(6) 0.004(5) C34 0.054(6) 0.033(5) 0.068(7) -0.003(5) 0.015(5) -0.003(5) C35 0.063(6) 0.047(6) 0.041(6) 0.006(5) -0.002(5) -0.001(5) C36 0.069(7) 0.050(6) 0.034(5) -0.001(5) 0.025(5) 0.000(5) P1 0.0476(16) 0.0652(17) 0.0563(18) -0.0002(14) 0.0185(15) -0.0077(14) F1 0.145(8) 0.175(9) 0.214(10) 0.083(8) 0.131(8) 0.083(7) F2 0.154(7) 0.163(8) 0.072(5) -0.015(5) 0.044(5) -0.052(6) F3 0.129(7) 0.160(9) 0.243(12) 0.111(9) 0.086(8) 0.079(7) F4 0.200(9) 0.198(10) 0.060(5) -0.021(6) 0.031(6) -0.122(8) F5 0.143(7) 0.088(5) 0.129(6) -0.013(5) 0.074(6) -0.046(5) F6 0.158(7) 0.124(7) 0.109(6) -0.015(5) 0.050(6) -0.090(6) P2 0.0625(16) 0.0305(12) 0.0367(13) 0.0035(11) 0.0228(12) 0.0074(13) F7 0.053(11) 0.32(4) 0.060(13) -0.12(2) -0.004(10) -0.05(2) F8 0.112(19) 0.026(10) 0.27(4) 0.014(15) 0.08(2) 0.037(11) F9 0.074(15) 0.20(3) 0.091(18) -0.10(2) 0.029(14) -0.034(19) F10 0.13(2) 0.028(11) 0.32(5) 0.040(19) 0.03(3) 0.065(13) F7A 0.103(11) 0.124(14) 0.072(10) 0.037(10) 0.003(9) 0.009(10) F8A 0.38(4) 0.086(13) 0.056(10) -0.030(9) 0.051(16) -0.123(18) F9A 0.093(12) 0.31(3) 0.095(13) 0.117(17) 0.028(12) 0.084(17) F10A 0.55(5) 0.045(10) 0.081(13) -0.017(8) 0.13(2) -0.039(18) F11 0.113(6) 0.174(8) 0.096(5) 0.050(6) 0.067(5) 0.023(5) F12 0.098(5) 0.127(6) 0.062(4) 0.015(4) 0.041(4) -0.031(4) C1S 0.105(11) 0.092(11) 0.096(11) -0.007(9) 0.015(9) 0.024(8) N1S 0.057(6) 0.102(9) 0.082(8) 0.033(8) -0.006(6) 0.000(6) O1S 0.151(11) 0.162(11) 0.125(9) 0.010(8) 0.058(8) -0.024(9) O2S 0.143(9) 0.079(7) 0.096(7) -0.014(6) -0.025(6) 0.015(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.160(7) . ? Ru1 C8 2.196(8) . ? Ru1 C7 2.205(8) . ? Ru1 C11 2.211(8) . ? Ru1 C9 2.215(7) . ? Ru1 C12 2.225(8) . ? Ru1 C10 2.245(8) . ? Ru1 S2 2.343(2) . ? Ru1 S1 2.385(2) . ? S1 C1 1.835(9) . ? S2 C4 1.825(8) . ? S2 C5 1.833(11) . ? N1 C2 1.473(11) . ? N1 C3 1.491(11) . ? C1 C2 1.485(11) . ? C3 C4 1.499(11) . ? C5 C6 1.478(15) . ? C6 C13 1.573(13) . ? C7 C12 1.403(11) . ? C7 C8 1.445(12) . ? C7 C13 1.522(12) . ? C8 C9 1.388(12) . ? C8 C14 1.517(11) . ? C9 C10 1.442(11) . ? C9 C15 1.511(11) . ? C10 C11 1.388(12) . ? C10 C16 1.510(12) . ? C11 C12 1.439(13) . ? C11 C17 1.530(11) . ? C12 C18 1.520(12) . ? Ru2 N2 2.151(7) . ? Ru2 C30 2.202(7) . ? Ru2 C25 2.203(8) . ? Ru2 C27 2.213(7) . ? Ru2 C29 2.217(7) . ? Ru2 C28 2.226(8) . ? Ru2 C26 2.227(7) . ? Ru2 S4 2.333(2) . ? Ru2 S3 2.387(2) . ? S3 C19 1.834(8) . ? S4 C23 1.803(9) . ? S4 C22 1.822(9) . ? N2 C20 1.483(11) . ? N2 C21 1.484(11) . ? C19 C20 1.518(11) . ? C21 C22 1.486(12) . ? C23 C24 1.525(13) . ? C24 C31 1.544(12) . ? C25 C30 1.430(11) . ? C25 C26 1.441(10) . ? C25 C31 1.517(11) . ? C26 C27 1.400(11) . ? C26 C32 1.506(11) . ? C27 C28 1.444(11) . ? C27 C33 1.518(10) . ? C28 C29 1.411(10) . ? C28 C34 1.504(11) . ? C29 C30 1.426(11) . ? C29 C35 1.516(11) . ? C30 C36 1.510(10) . ? P1 F3 1.540(3) . ? P1 F4 1.541(3) . ? P1 F1 1.543(3) . ? P1 F6 1.546(3) . ? P1 F5 1.547(3) . ? P1 F2 1.549(3) . ? P2 F8A 1.540(3) . ? P2 F8 1.541(3) . ? P2 F7 1.542(3) . ? P2 F9A 1.543(3) . ? P2 F10A 1.544(3) . ? P2 F9 1.544(3) . ? P2 F10 1.544(3) . ? P2 F7A 1.545(3) . ? P2 F12 1.546(3) . ? P2 F11 1.547(3) . ? C1S N1S 1.492(16) . ? N1S O1S 1.144(12) . ? N1S O2S 1.225(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 N1 Ru1 C8 162.5(3) . . ? N1 Ru1 C7 124.2(3) . . ? C8 Ru1 C7 38.3(3) . . ? N1 Ru1 C11 92.9(3) . . ? C8 Ru1 C11 79.8(3) . . ? C7 Ru1 C11 67.4(3) . . ? N1 Ru1 C9 152.2(3) . . ? C8 Ru1 C9 36.7(3) . . ? C7 Ru1 C9 67.5(3) . . ? C11 Ru1 C9 67.2(3) . . ? N1 Ru1 C12 96.6(3) . . ? C8 Ru1 C12 67.8(3) . . ? C7 Ru1 C12 36.9(3) . . ? C11 Ru1 C12 37.9(3) . . ? C9 Ru1 C12 79.7(3) . . ? N1 Ru1 C10 115.5(3) . . ? C8 Ru1 C10 66.9(3) . . ? C7 Ru1 C10 79.0(3) . . ? C11 Ru1 C10 36.3(3) . . ? C9 Ru1 C10 37.7(3) . . ? C12 Ru1 C10 66.7(3) . . ? N1 Ru1 S2 84.1(2) . . ? C8 Ru1 S2 95.6(2) . . ? C7 Ru1 S2 93.2(2) . . ? C11 Ru1 S2 154.3(3) . . ? C9 Ru1 S2 122.4(2) . . ? C12 Ru1 S2 117.0(3) . . ? C10 Ru1 S2 160.1(2) . . ? N1 Ru1 S1 82.6(2) . . ? C8 Ru1 S1 114.8(2) . . ? C7 Ru1 S1 152.8(2) . . ? C11 Ru1 S1 120.7(3) . . ? C9 Ru1 S1 91.0(2) . . ? C12 Ru1 S1 158.5(3) . . ? C10 Ru1 S1 94.1(2) . . ? S2 Ru1 S1 84.39(10) . . ? C1 S1 Ru1 100.8(3) . . ? C4 S2 C5 103.1(5) . . ? C4 S2 Ru1 100.6(3) . . ? C5 S2 Ru1 111.5(4) . . ? C2 N1 C3 114.8(7) . . ? C2 N1 Ru1 113.1(5) . . ? C3 N1 Ru1 113.0(5) . . ? C2 C1 S1 111.3(6) . . ? N1 C2 C1 113.5(7) . . ? N1 C3 C4 112.1(7) . . ? C3 C4 S2 112.0(6) . . ? C6 C5 S2 118.2(7) . . ? C5 C6 C13 116.2(11) . . ? C12 C7 C8 120.0(8) . . ? C12 C7 C13 119.4(9) . . ? C8 C7 C13 120.5(8) . . ? C12 C7 Ru1 72.3(5) . . ? C8 C7 Ru1 70.5(5) . . ? C13 C7 Ru1 127.9(6) . . ? C9 C8 C7 120.2(7) . . ? C9 C8 C14 119.6(9) . . ? C7 C8 C14 120.3(9) . . ? C9 C8 Ru1 72.4(4) . . ? C7 C8 Ru1 71.2(4) . . ? C14 C8 Ru1 129.4(6) . . ? C8 C9 C10 119.9(8) . . ? C8 C9 C15 121.4(8) . . ? C10 C9 C15 118.7(8) . . ? C8 C9 Ru1 71.0(5) . . ? C10 C9 Ru1 72.3(4) . . ? C15 C9 Ru1 128.0(6) . . ? C11 C10 C9 119.9(8) . . ? C11 C10 C16 121.2(9) . . ? C9 C10 C16 118.7(9) . . ? C11 C10 Ru1 70.5(5) . . ? C9 C10 Ru1 70.0(4) . . ? C16 C10 Ru1 128.9(6) . . ? C10 C11 C12 120.7(7) . . ? C10 C11 C17 120.8(9) . . ? C12 C11 C17 118.5(9) . . ? C10 C11 Ru1 73.2(5) . . ? C12 C11 Ru1 71.6(5) . . ? C17 C11 Ru1 126.8(6) . . ? C7 C12 C11 119.1(8) . . ? C7 C12 C18 121.0(10) . . ? C11 C12 C18 119.9(9) . . ? C7 C12 Ru1 70.8(5) . . ? C11 C12 Ru1 70.6(5) . . ? C18 C12 Ru1 131.8(6) . . ? C7 C13 C6 113.3(7) . . ? N2 Ru2 C30 97.6(3) . . ? N2 Ru2 C25 127.4(3) . . ? C30 Ru2 C25 37.9(3) . . ? N2 Ru2 C27 148.4(3) . . ? C30 Ru2 C27 80.4(3) . . ? C25 Ru2 C27 67.9(3) . . ? N2 Ru2 C29 91.9(3) . . ? C30 Ru2 C29 37.6(3) . . ? C25 Ru2 C29 67.7(3) . . ? C27 Ru2 C29 67.2(3) . . ? N2 Ru2 C28 111.9(3) . . ? C30 Ru2 C28 68.1(3) . . ? C25 Ru2 C28 80.8(3) . . ? C27 Ru2 C28 38.0(3) . . ? C29 Ru2 C28 37.0(3) . . ? N2 Ru2 C26 165.1(3) . . ? C30 Ru2 C26 68.0(3) . . ? C25 Ru2 C26 37.9(3) . . ? C27 Ru2 C26 36.8(3) . . ? C29 Ru2 C26 79.1(3) . . ? C28 Ru2 C26 67.5(3) . . ? N2 Ru2 S4 84.1(2) . . ? C30 Ru2 S4 113.5(2) . . ? C25 Ru2 S4 91.4(2) . . ? C27 Ru2 S4 125.9(2) . . ? C29 Ru2 S4 150.2(2) . . ? C28 Ru2 S4 163.8(2) . . ? C26 Ru2 S4 97.7(2) . . ? N2 Ru2 S3 82.1(2) . . ? C30 Ru2 S3 161.4(2) . . ? C25 Ru2 S3 149.8(2) . . ? C27 Ru2 S3 90.1(2) . . ? C29 Ru2 S3 123.8(2) . . ? C28 Ru2 S3 94.6(2) . . ? C26 Ru2 S3 112.8(2) . . ? S4 Ru2 S3 85.00(8) . . ? C19 S3 Ru2 101.4(3) . . ? C23 S4 C22 101.2(4) . . ? C23 S4 Ru2 107.7(3) . . ? C22 S4 Ru2 99.8(3) . . ? C20 N2 C21 115.7(7) . . ? C20 N2 Ru2 111.7(5) . . ? C21 N2 Ru2 113.8(6) . . ? C20 C19 S3 109.8(5) . . ? N2 C20 C19 111.7(8) . . ? N2 C21 C22 112.0(7) . . ? C21 C22 S4 111.0(6) . . ? C24 C23 S4 110.7(6) . . ? C23 C24 C31 115.5(8) . . ? C30 C25 C26 119.4(7) . . ? C30 C25 C31 121.1(7) . . ? C26 C25 C31 119.6(8) . . ? C30 C25 Ru2 71.0(4) . . ? C26 C25 Ru2 71.9(4) . . ? C31 C25 Ru2 130.3(6) . . ? C27 C26 C25 120.4(7) . . ? C27 C26 C32 118.9(7) . . ? C25 C26 C32 120.7(8) . . ? C27 C26 Ru2 71.1(4) . . ? C25 C26 Ru2 70.1(4) . . ? C32 C26 Ru2 133.0(6) . . ? C26 C27 C28 120.8(7) . . ? C26 C27 C33 120.6(8) . . ? C28 C27 C33 118.5(8) . . ? C26 C27 Ru2 72.2(4) . . ? C28 C27 Ru2 71.5(4) . . ? C33 C27 Ru2 130.0(5) . . ? C29 C28 C27 118.3(8) . . ? C29 C28 C34 121.0(8) . . ? C27 C28 C34 120.7(7) . . ? C29 C28 Ru2 71.1(4) . . ? C27 C28 Ru2 70.5(4) . . ? C34 C28 Ru2 129.7(5) . . ? C28 C29 C30 122.0(8) . . ? C28 C29 C35 119.2(8) . . ? C30 C29 C35 118.8(7) . . ? C28 C29 Ru2 71.8(4) . . ? C30 C29 Ru2 70.6(4) . . ? C35 C29 Ru2 130.0(5) . . ? C29 C30 C25 119.1(7) . . ? C29 C30 C36 118.8(8) . . ? C25 C30 C36 122.1(8) . . ? C29 C30 Ru2 71.8(4) . . ? C25 C30 Ru2 71.1(4) . . ? C36 C30 Ru2 129.3(5) . . ? C25 C31 C24 117.6(7) . . ? F3 P1 F4 90.3(2) . . ? F3 P1 F1 179.5(2) . . ? F4 P1 F1 90.15(19) . . ? F3 P1 F6 90.17(19) . . ? F4 P1 F6 89.88(18) . . ? F1 P1 F6 89.83(19) . . ? F3 P1 F5 90.07(19) . . ? F4 P1 F5 90.59(19) . . ? F1 P1 F5 89.93(19) . . ? F6 P1 F5 179.5(3) . . ? F3 P1 F2 89.79(19) . . ? F4 P1 F2 179.8(3) . . ? F1 P1 F2 89.71(19) . . ? F6 P1 F2 90.04(19) . . ? F5 P1 F2 89.49(18) . . ? F8A P2 F8 43.6(5) . . ? F8A P2 F7 133.7(5) . . ? F8 P2 F7 90.2(2) . . ? F8A P2 F9A 90.2(2) . . ? F8 P2 F9A 133.7(5) . . ? F7 P2 F9A 136.1(5) . . ? F8A P2 F10A 179.8(3) . . ? F8 P2 F10A 136.3(5) . . ? F7 P2 F10A 46.1(5) . . ? F9A P2 F10A 90.0(2) . . ? F8A P2 F9 46.5(5) . . ? F8 P2 F9 90.0(2) . . ? F7 P2 F9 179.8(3) . . ? F9A P2 F9 43.7(5) . . ? F10A P2 F9 133.7(5) . . ? F8A P2 F10 136.2(5) . . ? F8 P2 F10 179.8(3) . . ? F7 P2 F10 90.0(2) . . ? F9A P2 F10 46.1(5) . . ? F10A P2 F10 43.9(5) . . ? F9 P2 F10 89.8(2) . . ? F8A P2 F7A 90.0(2) . . ? F8 P2 F7A 46.4(5) . . ? F7 P2 F7A 43.7(5) . . ? F9A P2 F7A 179.8(3) . . ? F10A P2 F7A 89.9(2) . . ? F9 P2 F7A 136.5(5) . . ? F10 P2 F7A 133.8(5) . . ? F8A P2 F12 90.09(17) . . ? F8 P2 F12 90.03(18) . . ? F7 P2 F12 89.96(18) . . ? F9A P2 F12 89.86(17) . . ? F10A P2 F12 89.96(18) . . ? F9 P2 F12 90.15(18) . . ? F10 P2 F12 90.01(18) . . ? F7A P2 F12 90.27(17) . . ? F8A P2 F11 90.03(18) . . ? F8 P2 F11 90.13(18) . . ? F7 P2 F11 90.04(18) . . ? F9A P2 F11 90.03(17) . . ? F10A P2 F11 89.92(17) . . ? F9 P2 F11 89.85(18) . . ? F10 P2 F11 89.83(18) . . ? F7A P2 F11 89.84(17) . . ? F12 P2 F11 179.83(19) . . ? O1S N1S O2S 125.1(15) . . ? O1S N1S C1S 120.6(14) . . ? O2S N1S C1S 114.2(12) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.416 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.125 #===END Complex 12 data_3002a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H33.50 F6 N1.50 P Ru S2' _chemical_formula_weight 605.14 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 18.3830(9) _cell_length_b 21.1216(11) _cell_length_c 12.5607(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.8320(10) _cell_angle_gamma 90.00 _cell_volume 4773.4(4) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3991 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 24.84 _exptl_crystal_description 'long rod' _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2472 _exptl_absorpt_coefficient_mu 0.956 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.7625 _exptl_absorpt_correction_T_max 0.8778 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27372 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8382 _reflns_number_gt 6665 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0494P)^2^+8.1821P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8382 _refine_ls_number_parameters 599 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1189 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.094 _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 0.18137(2) 0.670746(19) 0.25430(3) 0.02182(13) Uani 1 1 d . A . Ru2 Ru 0.22293(2) 0.331999(19) 0.23424(3) 0.02353(13) Uani 1 1 d . . . S1 S 0.10596(10) 0.73361(7) 0.34615(13) 0.0414(4) Uani 1 1 d . A . S2 S 0.27855(9) 0.73091(8) 0.35210(14) 0.0438(4) Uani 1 1 d . . . S3 S 0.12974(10) 0.28142(7) 0.10097(12) 0.0413(4) Uani 1 1 d . . . S4 S 0.30350(10) 0.26403(7) 0.16877(13) 0.0411(4) Uani 1 1 d . . . N1 N 0.1676(3) 0.7494(2) 0.1445(4) 0.0393(14) Uani 1 1 d . . . H1 H 0.174(4) 0.740(3) 0.088(5) 0.04(2) Uiso 1 1 d . . . N2 N 0.2059(3) 0.2522(2) 0.3323(4) 0.0309(11) Uani 1 1 d . . . H2 H 0.208(3) 0.266(3) 0.397(4) 0.027(15) Uiso 1 1 d . . . C1 C 0.0852(4) 0.8001(3) 0.2545(5) 0.058(2) Uani 1 1 d . . . H1A H 0.0339 0.8139 0.2513 0.070 Uiso 1 1 calc R A . H1B H 0.1182 0.8355 0.2821 0.070 Uiso 1 1 calc R . . C2 C 0.0947(5) 0.7830(3) 0.1446(5) 0.069(3) Uani 1 1 d . A . H2A H 0.0924 0.8216 0.1006 0.082 Uiso 1 1 calc R . . H2B H 0.0536 0.7556 0.1105 0.082 Uiso 1 1 calc R . . C3 C 0.2344(6) 0.7902(4) 0.1569(6) 0.081(3) Uani 1 1 d . A . H3A H 0.2204 0.8306 0.1202 0.098 Uiso 1 1 calc R . . H3B H 0.2707 0.7698 0.1208 0.098 Uiso 1 1 calc R . . C4 C 0.2698(5) 0.8025(4) 0.2725(6) 0.071(2) Uani 1 1 d . A . H4A H 0.2398 0.8333 0.3032 0.085 Uiso 1 1 calc R . . H4B H 0.3192 0.8210 0.2762 0.085 Uiso 1 1 calc R . . C5 C 0.3647(5) 0.7048(4) 0.3068(8) 0.041(2) Uani 0.70 1 d PD A 1 H5A H 0.3573 0.7083 0.2275 0.049 Uiso 0.70 1 calc PR A 1 H5B H 0.4064 0.7322 0.3393 0.049 Uiso 0.70 1 calc PR A 1 C5A C 0.3574(11) 0.6881(9) 0.4022(15) 0.039(5) Uani 0.30 1 d PD A 2 H5A1 H 0.3984 0.7185 0.4202 0.047 Uiso 0.30 1 calc PR A 2 H5A2 H 0.3510 0.6694 0.4711 0.047 Uiso 0.30 1 calc PR A 2 C6 C 0.3824(3) 0.6380(3) 0.3403(7) 0.056(2) Uani 1 1 d D . . H6A H 0.3717 0.6361 0.4143 0.068 Uiso 0.70 1 calc PR A 1 H6A H 0.3806 0.6635 0.2737 0.068 Uiso 0.30 1 d PR A 2 C7 C 0.4653(4) 0.6245(4) 0.3597(6) 0.058(2) Uani 1 1 d . A . H7A H 0.4923 0.6587 0.4019 0.087 Uiso 1 1 calc R . . H7B H 0.4805 0.6213 0.2904 0.087 Uiso 1 1 calc R . . H7C H 0.4759 0.5850 0.3992 0.087 Uiso 1 1 calc R . . C8 C 0.2545(3) 0.5880(2) 0.2536(4) 0.0259(12) Uani 1 1 d . . . C9 C 0.2175(3) 0.6009(2) 0.1437(4) 0.0246(12) Uani 1 1 d . A . C10 C 0.1381(3) 0.6049(2) 0.1191(4) 0.0238(12) Uani 1 1 d . . . C11 C 0.0959(3) 0.5973(2) 0.2002(4) 0.0292(13) Uani 1 1 d . A . C12 C 0.1334(3) 0.5836(2) 0.3102(4) 0.0299(13) Uani 1 1 d . . . C13 C 0.2114(3) 0.5782(2) 0.3360(4) 0.0284(13) Uani 1 1 d . A . C14 C 0.3389(3) 0.5826(3) 0.2829(5) 0.0410(15) Uani 1 1 d . A . H14A H 0.3513 0.5451 0.3290 0.049 Uiso 1 1 calc R . . H14B H 0.3566 0.5747 0.2156 0.049 Uiso 1 1 calc R . . C15 C 0.2597(4) 0.6118(3) 0.0535(5) 0.0420(16) Uani 1 1 d . . . H15A H 0.3125 0.6144 0.0843 0.063 Uiso 1 1 calc R A . H15B H 0.2431 0.6511 0.0162 0.063 Uiso 1 1 calc R . . H15C H 0.2503 0.5770 0.0022 0.063 Uiso 1 1 calc R . . C16 C 0.0978(4) 0.6179(3) 0.0031(4) 0.0412(15) Uani 1 1 d . A . H16A H 0.0886 0.5782 -0.0363 0.062 Uiso 1 1 calc R . . H16B H 0.1281 0.6451 -0.0323 0.062 Uiso 1 1 calc R . . H16C H 0.0508 0.6387 0.0039 0.062 Uiso 1 1 calc R . . C17 C 0.0118(3) 0.6034(3) 0.1745(6) 0.0477(17) Uani 1 1 d . . . H17A H -0.0031 0.6333 0.1154 0.072 Uiso 1 1 calc R A . H17B H -0.0049 0.6184 0.2384 0.072 Uiso 1 1 calc R . . H17C H -0.0102 0.5624 0.1532 0.072 Uiso 1 1 calc R . . C18 C 0.0878(4) 0.5746(3) 0.3962(5) 0.0486(18) Uani 1 1 d . A . H18A H 0.1206 0.5659 0.4656 0.073 Uiso 1 1 calc R . . H18B H 0.0539 0.5394 0.3763 0.073 Uiso 1 1 calc R . . H18C H 0.0597 0.6128 0.4021 0.073 Uiso 1 1 calc R . . C19 C 0.2500(4) 0.5606(3) 0.4508(4) 0.0450(17) Uani 1 1 d . . . H19A H 0.2513 0.5971 0.4980 0.068 Uiso 1 1 calc R A . H19B H 0.3003 0.5468 0.4508 0.068 Uiso 1 1 calc R . . H19C H 0.2229 0.5265 0.4770 0.068 Uiso 1 1 calc R . . C20 C 0.1106(3) 0.2116(3) 0.1755(5) 0.0368(14) Uani 1 1 d . . . H20A H 0.0577 0.2010 0.1545 0.044 Uiso 1 1 calc R . . H20B H 0.1392 0.1757 0.1565 0.044 Uiso 1 1 calc R . . C21 C 0.1307(3) 0.2227(3) 0.2962(5) 0.0367(14) Uani 1 1 d . . . H21A H 0.0933 0.2504 0.3174 0.044 Uiso 1 1 calc R . . H21B H 0.1296 0.1822 0.3339 0.044 Uiso 1 1 calc R . . C22 C 0.2683(3) 0.2063(3) 0.3478(4) 0.0377(15) Uani 1 1 d . . . H22A H 0.2526 0.1668 0.3772 0.045 Uiso 1 1 calc R . . H22B H 0.3101 0.2234 0.4013 0.045 Uiso 1 1 calc R . . C23 C 0.2938(4) 0.1922(3) 0.2439(5) 0.0415(15) Uani 1 1 d . . . H23A H 0.2579 0.1641 0.1986 0.050 Uiso 1 1 calc R . . H23B H 0.3418 0.1702 0.2610 0.050 Uiso 1 1 calc R . . C24 C 0.4006(4) 0.2867(3) 0.2162(6) 0.056(2) Uani 1 1 d . . . H24A H 0.4293 0.2474 0.2307 0.067 Uiso 1 1 calc R . . H24B H 0.4166 0.3074 0.1550 0.067 Uiso 1 1 calc R . . C25 C 0.4244(3) 0.3283(3) 0.3128(5) 0.0418(15) Uani 1 1 d . . . H25 H 0.4081 0.3085 0.3754 0.050 Uiso 1 1 calc R . . C26 C 0.5094(4) 0.3317(4) 0.3389(7) 0.060(2) Uani 1 1 d . . . H26A H 0.5296 0.2902 0.3608 0.090 Uiso 1 1 calc R . . H26B H 0.5256 0.3616 0.3977 0.090 Uiso 1 1 calc R . . H26C H 0.5269 0.3455 0.2749 0.090 Uiso 1 1 calc R . . C27 C 0.3102(3) 0.4040(2) 0.2844(4) 0.0274(12) Uani 1 1 d . . . C28 C 0.2742(3) 0.3950(2) 0.3716(4) 0.0258(12) Uani 1 1 d . . . C29 C 0.1948(3) 0.3989(2) 0.3533(4) 0.0293(13) Uani 1 1 d . . . C30 C 0.1521(3) 0.4158(2) 0.2501(4) 0.0288(13) Uani 1 1 d . . . C31 C 0.1896(3) 0.4253(2) 0.1610(4) 0.0282(13) Uani 1 1 d . . . C32 C 0.2674(3) 0.4197(2) 0.1773(4) 0.0255(12) Uani 1 1 d . . . C33 C 0.3936(3) 0.3966(3) 0.3003(5) 0.0379(14) Uani 1 1 d . . . H33A H 0.4167 0.4206 0.3652 0.046 Uiso 1 1 calc R . . H33B H 0.4095 0.4161 0.2380 0.046 Uiso 1 1 calc R . . C34 C 0.3180(4) 0.3814(3) 0.4850(4) 0.0406(16) Uani 1 1 d . . . H34A H 0.3705 0.3879 0.4871 0.061 Uiso 1 1 calc R . . H34B H 0.3096 0.3380 0.5043 0.061 Uiso 1 1 calc R . . H34C H 0.3018 0.4098 0.5363 0.061 Uiso 1 1 calc R . . C35 C 0.1566(4) 0.3849(3) 0.4465(5) 0.0404(15) Uani 1 1 d . . . H35A H 0.1506 0.4239 0.4845 0.061 Uiso 1 1 calc R . . H35B H 0.1864 0.3554 0.4963 0.061 Uiso 1 1 calc R . . H35C H 0.1081 0.3665 0.4183 0.061 Uiso 1 1 calc R . . C36 C 0.0688(3) 0.4216(3) 0.2300(5) 0.0434(16) Uani 1 1 d . . . H36A H 0.0522 0.4151 0.2977 0.065 Uiso 1 1 calc R . . H36B H 0.0464 0.3900 0.1775 0.065 Uiso 1 1 calc R . . H36C H 0.0542 0.4635 0.2020 0.065 Uiso 1 1 calc R . . C37 C 0.1430(4) 0.4403(3) 0.0500(5) 0.0442(16) Uani 1 1 d . . . H37A H 0.1532 0.4832 0.0298 0.066 Uiso 1 1 calc R . . H37B H 0.0908 0.4363 0.0520 0.066 Uiso 1 1 calc R . . H37C H 0.1553 0.4109 -0.0031 0.066 Uiso 1 1 calc R . . C38 C 0.3051(4) 0.4307(3) 0.0825(5) 0.0412(16) Uani 1 1 d . . . H38A H 0.2679 0.4332 0.0157 0.062 Uiso 1 1 calc R . . H38B H 0.3388 0.3959 0.0777 0.062 Uiso 1 1 calc R . . H38C H 0.3329 0.4700 0.0934 0.062 Uiso 1 1 calc R . . P1 P 0.16580(10) 0.49685(7) 0.73514(12) 0.0346(4) Uani 1 1 d . . . F1 F 0.1625(5) 0.5611(2) 0.6757(5) 0.159(4) Uani 1 1 d . . . F2 F 0.2270(3) 0.5224(4) 0.8291(4) 0.134(3) Uani 1 1 d . . . F3 F 0.1692(4) 0.4325(2) 0.7934(4) 0.116(2) Uani 1 1 d . . . F4 F 0.1045(3) 0.4693(3) 0.6429(4) 0.107(2) Uani 1 1 d . . . F5 F 0.1064(3) 0.5196(2) 0.8020(3) 0.0719(13) Uani 1 1 d . . . F6 F 0.2263(2) 0.4725(2) 0.6704(3) 0.0723(13) Uani 1 1 d . . . P2 P 0.51917(10) 0.35237(9) 0.97754(14) 0.0455(4) Uani 1 1 d . . . F7 F 0.5504(2) 0.41593(19) 0.9382(3) 0.0621(11) Uani 1 1 d . . . F8 F 0.4611(3) 0.3483(3) 0.8686(5) 0.130(3) Uani 1 1 d . . . F9 F 0.4870(3) 0.2875(2) 1.0144(4) 0.0770(14) Uani 1 1 d . . . F10 F 0.5784(3) 0.3550(3) 1.0856(4) 0.1060(19) Uani 1 1 d . . . F11 F 0.4651(3) 0.3917(2) 1.0326(5) 0.113(2) Uani 1 1 d . . . F12 F 0.5753(3) 0.3128(2) 0.9260(5) 0.0934(17) Uani 1 1 d . . . N1S N 0.4153(6) 0.5156(5) 0.5974(10) 0.111(4) Uani 1 1 d . . . C1S C 0.4111(6) 0.5089(4) 0.6837(12) 0.086(4) Uani 1 1 d . . . C2S C 0.4036(6) 0.5013(5) 0.7960(10) 0.101(3) Uani 1 1 d . . . H2S1 H 0.4429 0.5246 0.8434 0.152 Uiso 1 1 calc R . . H2S2 H 0.4073 0.4568 0.8152 0.152 Uiso 1 1 calc R . . H2S3 H 0.3557 0.5175 0.8043 0.152 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 0.0295(3) 0.0167(2) 0.0193(2) -0.00114(17) 0.00500(18) 0.00078(18) Ru2 0.0358(3) 0.0165(2) 0.0186(2) -0.00073(17) 0.00630(19) -0.00299(19) S1 0.0535(11) 0.0289(8) 0.0493(10) -0.0044(7) 0.0279(8) 0.0049(7) S2 0.0422(10) 0.0301(9) 0.0526(10) -0.0151(7) -0.0049(8) -0.0003(7) S3 0.0631(11) 0.0294(8) 0.0260(8) 0.0010(6) -0.0035(7) -0.0162(8) S4 0.0570(11) 0.0285(8) 0.0425(9) -0.0055(7) 0.0211(8) 0.0026(7) N1 0.071(4) 0.027(3) 0.020(3) 0.004(2) 0.009(3) 0.003(3) N2 0.052(3) 0.022(3) 0.018(2) -0.001(2) 0.007(2) -0.002(2) C1 0.077(5) 0.041(4) 0.056(4) 0.012(3) 0.013(4) 0.031(4) C2 0.113(7) 0.045(4) 0.038(4) 0.004(3) -0.007(4) 0.048(5) C3 0.147(9) 0.046(5) 0.059(5) -0.003(4) 0.042(5) -0.050(5) C4 0.091(7) 0.048(5) 0.077(6) -0.007(4) 0.023(5) -0.027(4) C5 0.031(5) 0.037(5) 0.058(6) -0.017(5) 0.016(4) -0.006(4) C5A 0.044(13) 0.041(12) 0.032(11) -0.014(9) 0.005(9) -0.025(10) C6 0.028(4) 0.047(4) 0.094(6) -0.005(4) 0.011(4) 0.001(3) C7 0.034(4) 0.068(5) 0.072(5) -0.005(4) 0.009(4) 0.002(4) C8 0.031(3) 0.014(3) 0.029(3) -0.006(2) -0.002(2) 0.005(2) C9 0.036(3) 0.013(2) 0.025(3) -0.006(2) 0.007(2) -0.002(2) C10 0.033(3) 0.014(3) 0.022(3) -0.003(2) 0.000(2) 0.002(2) C11 0.033(3) 0.014(3) 0.041(3) -0.004(2) 0.009(3) -0.006(2) C12 0.055(4) 0.018(3) 0.019(3) 0.000(2) 0.012(3) -0.004(3) C13 0.044(4) 0.016(3) 0.025(3) 0.003(2) 0.005(3) 0.002(2) C14 0.039(4) 0.041(4) 0.039(4) -0.011(3) -0.001(3) 0.004(3) C15 0.051(4) 0.044(4) 0.034(3) -0.012(3) 0.017(3) -0.008(3) C16 0.053(4) 0.034(3) 0.030(3) -0.001(3) -0.006(3) 0.008(3) C17 0.035(4) 0.046(4) 0.059(4) -0.006(3) 0.003(3) -0.007(3) C18 0.067(5) 0.039(4) 0.048(4) 0.005(3) 0.031(4) -0.002(3) C19 0.070(5) 0.032(3) 0.029(3) 0.004(3) 0.001(3) -0.001(3) C20 0.041(4) 0.032(3) 0.039(3) -0.007(3) 0.012(3) -0.013(3) C21 0.043(4) 0.031(3) 0.039(3) 0.005(3) 0.015(3) -0.005(3) C22 0.050(4) 0.026(3) 0.030(3) 0.006(3) -0.007(3) -0.001(3) C23 0.040(4) 0.028(3) 0.056(4) -0.007(3) 0.008(3) 0.002(3) C24 0.056(5) 0.039(4) 0.083(5) 0.001(4) 0.037(4) 0.003(3) C25 0.037(4) 0.047(4) 0.042(4) 0.005(3) 0.008(3) -0.003(3) C26 0.035(4) 0.055(5) 0.087(6) 0.006(4) 0.009(4) 0.005(3) C27 0.029(3) 0.016(3) 0.037(3) -0.001(2) 0.007(2) -0.006(2) C28 0.036(3) 0.019(3) 0.021(3) -0.003(2) 0.003(2) 0.000(2) C29 0.049(4) 0.018(3) 0.024(3) -0.006(2) 0.014(3) -0.005(3) C30 0.034(3) 0.016(3) 0.037(3) -0.006(2) 0.009(3) -0.002(2) C31 0.046(4) 0.013(3) 0.023(3) 0.006(2) 0.000(3) -0.006(2) C32 0.039(3) 0.015(3) 0.024(3) 0.001(2) 0.010(2) -0.004(2) C33 0.034(4) 0.030(3) 0.049(4) 0.003(3) 0.005(3) -0.001(3) C34 0.060(4) 0.037(4) 0.022(3) 0.001(3) 0.001(3) 0.002(3) C35 0.050(4) 0.041(4) 0.034(3) -0.007(3) 0.018(3) -0.006(3) C36 0.039(4) 0.034(4) 0.055(4) -0.002(3) 0.004(3) -0.004(3) C37 0.056(4) 0.037(4) 0.033(3) 0.009(3) -0.006(3) -0.003(3) C38 0.057(4) 0.033(3) 0.039(4) 0.005(3) 0.021(3) 0.002(3) P1 0.0595(11) 0.0244(8) 0.0221(8) -0.0027(6) 0.0138(7) -0.0053(7) F1 0.360(11) 0.047(3) 0.107(4) 0.035(3) 0.132(6) 0.035(5) F2 0.085(4) 0.237(8) 0.085(4) -0.091(5) 0.029(3) -0.060(5) F3 0.219(7) 0.059(3) 0.096(4) 0.032(3) 0.095(4) 0.050(4) F4 0.060(3) 0.180(6) 0.078(3) -0.068(4) 0.008(3) -0.001(3) F5 0.092(3) 0.069(3) 0.066(3) -0.019(2) 0.042(3) 0.017(3) F6 0.064(3) 0.104(4) 0.058(3) -0.032(2) 0.035(2) -0.021(3) P2 0.0422(10) 0.0537(11) 0.0443(10) 0.0047(8) 0.0175(8) 0.0031(9) F7 0.058(3) 0.056(3) 0.078(3) 0.010(2) 0.025(2) -0.006(2) F8 0.102(4) 0.155(6) 0.103(4) 0.042(4) -0.045(4) -0.068(4) F9 0.094(4) 0.063(3) 0.092(3) 0.016(2) 0.058(3) 0.000(3) F10 0.139(5) 0.088(4) 0.071(3) 0.000(3) -0.027(3) 0.017(4) F11 0.119(5) 0.070(3) 0.187(6) 0.035(4) 0.116(4) 0.034(3) F12 0.091(4) 0.069(3) 0.143(5) -0.029(3) 0.078(4) -0.014(3) N1S 0.086(7) 0.089(7) 0.139(9) 0.016(7) -0.024(7) -0.011(5) C1S 0.056(6) 0.045(5) 0.133(10) 0.001(7) -0.036(7) 0.001(4) C2S 0.075(7) 0.080(7) 0.136(10) -0.016(7) -0.011(7) 0.004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.141(5) . ? Ru1 C8 2.206(5) . ? Ru1 C10 2.212(5) . ? Ru1 C11 2.214(5) . ? Ru1 C12 2.218(5) . ? Ru1 C9 2.218(5) . ? Ru1 C13 2.223(5) . ? Ru1 S2 2.3270(16) . ? Ru1 S1 2.3817(15) . ? Ru2 N2 2.148(4) . ? Ru2 C29 2.195(5) . ? Ru2 C32 2.202(5) . ? Ru2 C27 2.207(5) . ? Ru2 C31 2.208(5) . ? Ru2 C28 2.228(5) . ? Ru2 C30 2.229(5) . ? Ru2 S4 2.3303(16) . ? Ru2 S3 2.3880(15) . ? S1 C1 1.806(6) . ? S2 C5A 1.72(2) . ? S2 C4 1.802(8) . ? S2 C5 1.873(8) . ? S3 C20 1.819(6) . ? S4 C23 1.814(6) . ? S4 C24 1.826(7) . ? N1 C3 1.481(9) . ? N1 C2 1.516(9) . ? N2 C22 1.483(7) . ? N2 C21 1.498(7) . ? C1 C2 1.472(9) . ? C3 C4 1.488(10) . ? C5 C6 1.489(10) . ? C5A C6 1.443(15) . ? C6 C14 1.513(9) . ? C6 C7 1.519(9) . ? C8 C9 1.435(7) . ? C8 C13 1.441(7) . ? C8 C14 1.523(8) . ? C9 C10 1.430(7) . ? C9 C15 1.516(7) . ? C10 C11 1.411(7) . ? C10 C16 1.518(7) . ? C11 C12 1.442(8) . ? C11 C17 1.517(8) . ? C12 C13 1.410(8) . ? C12 C18 1.508(7) . ? C13 C19 1.517(7) . ? C20 C21 1.504(8) . ? C22 C23 1.505(8) . ? C24 C25 1.490(9) . ? C25 C26 1.531(9) . ? C25 C33 1.546(8) . ? C27 C28 1.405(7) . ? C27 C32 1.451(7) . ? C27 C33 1.513(8) . ? C28 C29 1.433(8) . ? C28 C34 1.512(7) . ? C29 C30 1.415(8) . ? C29 C35 1.512(7) . ? C30 C31 1.443(7) . ? C30 C36 1.506(8) . ? C31 C32 1.408(8) . ? C31 C37 1.512(7) . ? C32 C38 1.514(7) . ? P1 F3 1.539(5) . ? P1 F1 1.544(5) . ? P1 F2 1.551(5) . ? P1 F4 1.554(5) . ? P1 F5 1.583(4) . ? P1 F6 1.592(4) . ? P2 F8 1.556(5) . ? P2 F10 1.557(5) . ? P2 F11 1.561(5) . ? P2 F12 1.567(5) . ? P2 F7 1.579(4) . ? P2 F9 1.598(5) . ? N1S C1S 1.112(14) . ? C1S C2S 1.453(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 C8 127.2(2) . . ? N1 Ru1 C10 90.99(19) . . ? C8 Ru1 C10 67.83(19) . . ? N1 Ru1 C11 111.3(2) . . ? C8 Ru1 C11 80.7(2) . . ? C10 Ru1 C11 37.18(19) . . ? N1 Ru1 C12 147.8(2) . . ? C8 Ru1 C12 68.0(2) . . ? C10 Ru1 C12 67.50(19) . . ? C11 Ru1 C12 38.0(2) . . ? N1 Ru1 C9 97.1(2) . . ? C8 Ru1 C9 37.85(19) . . ? C10 Ru1 C9 37.66(19) . . ? C11 Ru1 C9 68.1(2) . . ? C12 Ru1 C9 80.56(19) . . ? N1 Ru1 C13 164.7(2) . . ? C8 Ru1 C13 37.98(19) . . ? C10 Ru1 C13 79.53(19) . . ? C11 Ru1 C13 67.7(2) . . ? C12 Ru1 C13 37.0(2) . . ? C9 Ru1 C13 68.10(19) . . ? N1 Ru1 S2 83.84(16) . . ? C8 Ru1 S2 91.82(14) . . ? C10 Ru1 S2 149.82(15) . . ? C11 Ru1 S2 164.71(15) . . ? C12 Ru1 S2 126.78(15) . . ? C9 Ru1 S2 113.42(15) . . ? C13 Ru1 S2 98.33(15) . . ? N1 Ru1 S1 82.85(16) . . ? C8 Ru1 S1 149.24(14) . . ? C10 Ru1 S1 124.68(15) . . ? C11 Ru1 S1 95.29(15) . . ? C12 Ru1 S1 90.04(15) . . ? C9 Ru1 S1 162.26(15) . . ? C13 Ru1 S1 112.37(15) . . ? S2 Ru1 S1 84.26(6) . . ? N2 Ru2 C29 91.86(19) . . ? N2 Ru2 C32 162.48(19) . . ? C29 Ru2 C32 80.50(19) . . ? N2 Ru2 C27 124.06(19) . . ? C29 Ru2 C27 67.8(2) . . ? C32 Ru2 C27 38.42(19) . . ? N2 Ru2 C31 151.5(2) . . ? C29 Ru2 C31 67.99(19) . . ? C32 Ru2 C31 37.2(2) . . ? C27 Ru2 C31 68.1(2) . . ? N2 Ru2 C28 96.48(18) . . ? C29 Ru2 C28 37.8(2) . . ? C32 Ru2 C28 67.87(19) . . ? C27 Ru2 C28 36.93(19) . . ? C31 Ru2 C28 80.05(19) . . ? N2 Ru2 C30 114.53(19) . . ? C29 Ru2 C30 37.3(2) . . ? C32 Ru2 C30 67.9(2) . . ? C27 Ru2 C30 80.3(2) . . ? C31 Ru2 C30 38.0(2) . . ? C28 Ru2 C30 67.6(2) . . ? N2 Ru2 S4 84.06(14) . . ? C29 Ru2 S4 153.22(16) . . ? C32 Ru2 S4 95.65(14) . . ? C27 Ru2 S4 92.72(15) . . ? C31 Ru2 S4 123.03(15) . . ? C28 Ru2 S4 116.25(15) . . ? C30 Ru2 S4 160.98(15) . . ? N2 Ru2 S3 83.26(13) . . ? C29 Ru2 S3 122.01(16) . . ? C32 Ru2 S3 114.17(14) . . ? C27 Ru2 S3 152.09(15) . . ? C31 Ru2 S3 90.53(14) . . ? C28 Ru2 S3 159.78(15) . . ? C30 Ru2 S3 94.00(15) . . ? S4 Ru2 S3 83.89(6) . . ? C1 S1 Ru1 101.1(2) . . ? C5A S2 C4 128.2(7) . . ? C5A S2 C5 41.6(7) . . ? C4 S2 C5 93.7(4) . . ? C5A S2 Ru1 113.9(6) . . ? C4 S2 Ru1 101.2(3) . . ? C5 S2 Ru1 106.5(3) . . ? C20 S3 Ru2 100.86(19) . . ? C23 S4 C24 104.1(3) . . ? C23 S4 Ru2 101.2(2) . . ? C24 S4 Ru2 111.9(2) . . ? C3 N1 C2 116.2(6) . . ? C3 N1 Ru1 113.4(5) . . ? C2 N1 Ru1 110.5(4) . . ? C22 N2 C21 114.2(5) . . ? C22 N2 Ru2 112.8(4) . . ? C21 N2 Ru2 112.7(3) . . ? C2 C1 S1 110.9(5) . . ? C1 C2 N1 113.0(6) . . ? N1 C3 C4 113.0(6) . . ? C3 C4 S2 111.4(5) . . ? C6 C5 S2 110.1(6) . . ? C6 C5A S2 121.9(12) . . ? C5A C6 C5 51.8(9) . . ? C5A C6 C14 128.9(9) . . ? C5 C6 C14 122.3(7) . . ? C5A C6 C7 118.0(10) . . ? C5 C6 C7 112.1(6) . . ? C14 C6 C7 110.3(6) . . ? C9 C8 C13 119.7(5) . . ? C9 C8 C14 120.4(5) . . ? C13 C8 C14 119.9(5) . . ? C9 C8 Ru1 71.6(3) . . ? C13 C8 Ru1 71.7(3) . . ? C14 C8 Ru1 130.6(4) . . ? C10 C9 C8 118.7(5) . . ? C10 C9 C15 119.0(5) . . ? C8 C9 C15 122.3(5) . . ? C10 C9 Ru1 70.9(3) . . ? C8 C9 Ru1 70.6(3) . . ? C15 C9 Ru1 129.2(4) . . ? C11 C10 C9 121.7(5) . . ? C11 C10 C16 118.7(5) . . ? C9 C10 C16 119.6(5) . . ? C11 C10 Ru1 71.5(3) . . ? C9 C10 Ru1 71.4(3) . . ? C16 C10 Ru1 130.6(4) . . ? C10 C11 C12 119.3(5) . . ? C10 C11 C17 121.6(5) . . ? C12 C11 C17 119.1(5) . . ? C10 C11 Ru1 71.4(3) . . ? C12 C11 Ru1 71.2(3) . . ? C17 C11 Ru1 129.3(4) . . ? C13 C12 C11 120.0(5) . . ? C13 C12 C18 120.9(5) . . ? C11 C12 C18 119.0(5) . . ? C13 C12 Ru1 71.7(3) . . ? C11 C12 Ru1 70.9(3) . . ? C18 C12 Ru1 130.3(4) . . ? C12 C13 C8 120.5(5) . . ? C12 C13 C19 119.6(5) . . ? C8 C13 C19 120.0(5) . . ? C12 C13 Ru1 71.3(3) . . ? C8 C13 Ru1 70.3(3) . . ? C19 C13 Ru1 132.7(4) . . ? C6 C14 C8 118.0(5) . . ? C21 C20 S3 111.1(4) . . ? N2 C21 C20 113.0(5) . . ? N2 C22 C23 112.7(5) . . ? C22 C23 S4 111.5(4) . . ? C25 C24 S4 121.6(5) . . ? C24 C25 C26 108.6(6) . . ? C24 C25 C33 115.3(5) . . ? C26 C25 C33 108.3(5) . . ? C28 C27 C32 120.0(5) . . ? C28 C27 C33 120.7(5) . . ? C32 C27 C33 119.2(5) . . ? C28 C27 Ru2 72.4(3) . . ? C32 C27 Ru2 70.6(3) . . ? C33 C27 Ru2 128.7(4) . . ? C27 C28 C29 119.7(5) . . ? C27 C28 C34 121.0(5) . . ? C29 C28 C34 119.3(5) . . ? C27 C28 Ru2 70.7(3) . . ? C29 C28 Ru2 69.8(3) . . ? C34 C28 Ru2 132.5(4) . . ? C30 C29 C28 121.1(5) . . ? C30 C29 C35 120.0(5) . . ? C28 C29 C35 118.9(5) . . ? C30 C29 Ru2 72.6(3) . . ? C28 C29 Ru2 72.4(3) . . ? C35 C29 Ru2 127.8(4) . . ? C29 C30 C31 118.9(5) . . ? C29 C30 C36 121.8(5) . . ? C31 C30 C36 119.3(5) . . ? C29 C30 Ru2 70.0(3) . . ? C31 C30 Ru2 70.2(3) . . ? C36 C30 Ru2 130.0(4) . . ? C32 C31 C30 120.5(5) . . ? C32 C31 C37 121.2(5) . . ? C30 C31 C37 118.4(5) . . ? C32 C31 Ru2 71.1(3) . . ? C30 C31 Ru2 71.8(3) . . ? C37 C31 Ru2 128.8(4) . . ? C31 C32 C27 119.8(5) . . ? C31 C32 C38 119.2(5) . . ? C27 C32 C38 121.0(5) . . ? C31 C32 Ru2 71.6(3) . . ? C27 C32 Ru2 71.0(3) . . ? C38 C32 Ru2 130.2(4) . . ? C27 C33 C25 116.7(5) . . ? F3 P1 F1 179.4(3) . . ? F3 P1 F2 89.6(4) . . ? F1 P1 F2 90.7(4) . . ? F3 P1 F4 88.7(4) . . ? F1 P1 F4 91.0(4) . . ? F2 P1 F4 178.3(4) . . ? F3 P1 F5 89.0(3) . . ? F1 P1 F5 91.5(3) . . ? F2 P1 F5 87.8(3) . . ? F4 P1 F5 92.0(3) . . ? F3 P1 F6 89.6(3) . . ? F1 P1 F6 89.9(3) . . ? F2 P1 F6 91.6(3) . . ? F4 P1 F6 88.5(2) . . ? F5 P1 F6 178.4(3) . . ? F8 P2 F10 178.5(4) . . ? F8 P2 F11 92.0(4) . . ? F10 P2 F11 89.4(3) . . ? F8 P2 F12 89.9(4) . . ? F10 P2 F12 88.7(3) . . ? F11 P2 F12 178.1(4) . . ? F8 P2 F7 90.0(3) . . ? F10 P2 F7 90.5(3) . . ? F11 P2 F7 89.5(3) . . ? F12 P2 F7 90.7(2) . . ? F8 P2 F9 88.8(3) . . ? F10 P2 F9 90.7(3) . . ? F11 P2 F9 91.2(3) . . ? F12 P2 F9 88.6(3) . . ? F7 P2 F9 178.6(3) . . ? N1S C1S C2S 178.3(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.919 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.120 #===END