Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #=================================================================== _audit_creation_date 'July 21 2004' _audit_creation_method 'from NRCVAX CIF routine and SHELXL97 with Word-Perfect' _audit_update_record ; July 23 2004 Assembled from individual CIFs for 1, 2 and 4 All three structures give no A-alerts with PLATON Check.def ; #=================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Trevor R. Spalding ; _publ_contact_author_phone ? _publ_contact_author_fax ? _publ_contact_author_email t.spalding@ucc.ie #===================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Metallaheteroborane Chemistry Part 17.1 Coordination and Cluster Compounds of Ruthenium with the [hypho-1,2-S2B6H9]- ligand ; loop_ _publ_author_name _publ_author_address G.Ferguson ; School of Chemistry, University of St. Andrews, St. Andrews, Fife, KY16 9SH, Scotland ; J.F.Gallagher ; Department of Chemistry Dublin City University Dublin, Ireland ; J.D.Kennedy ; Department of Chemistry University of Leeds, Leeds LS2 9JT, England ; D.McCarthy ; Department of Chemistry University College Cork National University of Ireland, Cork, Ireland ; T.R.Spalding ; Department of Chemistry University College Cork National University of Ireland, Cork, Ireland Dublin, Ireland ; #====================================================================== _publ_section_exptl_refinement ; ; _publ_section_references ; Flack, H. (1983). Acta Cryst. A39, 876--881. Gabe, E.J., Le Page, Y., Charland,.J.-P., Lee, F.L. & White, P.S. (1989). J. Appl. Cryst. 22, 384--387. Gabe, E.J. & White, P.S. (1993). DIFRAC - a diffractometer control program. Anerican Crystallographic Association, Pittsburgh Meeting, Abstract XXX. Johnson, C.K. (1976). ORTEP - A Fortran Thermal Ellipsoid Plot Program, Technical Report ORNL-5138, Oak Ridge National Laboratory, U.S.A. North, A.C.T., Phillips, D.C. & Mathews, F.S. (1968). Acta Cryst. A24, 351--359. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. Univ. of G\"ottingen, Germany. Spek, A.L. (2003). PLATON Molecular Geometry Program, University of Utrecht, Utrecht, Holland. ; _publ_contact_author_name 'Trevor R. Spalding' #===================================================================== data_compd-1 _database_code_depnum_ccdc_archive 'CCDC 264502' #===================================================================== # 5. Chemical Data _chemical_name_systematic ; ? #Insert the chemical name here. ; _chemical_name_common ? _chemical_formula_moiety 'C23 H29 B6 P Ru S2 ' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C23 H29 B6 P Ru S2' _chemical_formula_weight 566.50 _chemical_compound_source 'synthesized by the authors, see text' 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' B B 0.0013 0.0007 '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' 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' #========================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P c' _symmetry_space_group_name_Hall 'P -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 9.482(2) _cell_length_b 14.275(5) _cell_length_c 9.753(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.49(2) _cell_angle_gamma 90.00 _cell_volume 1317.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 294(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.00 _cell_measurement_theta_max 19.90 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description 'triangular block' _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method ? _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type psi-scan # 3 psi-scans at 4\% steps (North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.683 _exptl_absorpt_correction_T_max 0.848 _exptl_absorpt_process_details 'North et al., 1968' #========================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? #Insert any special details here. ; _diffrn_ambient_temperature 294(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 10.1 _diffrn_reflns_number 3036 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.50 #26.91 _reflns_number_total 3036 _reflns_number_observed 2707 _reflns_observed_criterion >2\s(I) _computing_data_collection 'DIFRAC (Gabe & White, 1993)' _computing_cell_refinement 'DIFRAC (Gabe & White, 1993)' _computing_data_reduction 'DATRD2 in NRCVAX94 (Gabe, Le Page, Charland, Lee & White, 1989)' _computing_structure_solution 'Patterson heavy-atom method and NRCVAX94' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'NRCVAX94, SHELXL97' #========================================================================= _refine_special_details ; Compound 1 crystallised in the monoclinic system; space group Pc or P2/c from the systematic absences; Pc assumed and confirmed by the analysis. All H atoms were clearly revealed in difference maps. The bridging H atoms in the boron cage were refined with restraints [B-H 1.24(4)\%A] and the terminal B-H atoms were refined with B-H 1.10(4)\%A restraints. All other H atoms were allowed for as riding with the normal SHELXL-97 constraints. ; # 8. Refinement Data _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^)+(0.0758P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(4) _refine_ls_number_reflns 3036 _refine_ls_number_parameters 325 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.995 _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 Ru5 Ru 0.50000(2) 0.27739(2) 0.50000(2) 0.03283(11) Uani 1 1 d . . . P1 P 0.42912(14) 0.22746(8) 0.28223(13) 0.0327(3) Uani 1 1 d . . . S4 S 0.61531(14) 0.41224(9) 0.41215(14) 0.0393(3) Uani 1 1 d . . . S6 S 0.71359(15) 0.18787(9) 0.50062(15) 0.0419(3) Uani 1 1 d . . . B1 B 0.8011(7) 0.3755(5) 0.3652(7) 0.0430(13) Uani 1 1 d D . . B2 B 0.8523(7) 0.2579(5) 0.4106(8) 0.0442(13) Uani 1 1 d D . . B3 B 0.9085(6) 0.3551(5) 0.5182(7) 0.0431(13) Uani 1 1 d D . . B7 B 0.8526(7) 0.2524(5) 0.6123(7) 0.0476(14) Uani 1 1 d D . . B8 B 0.8364(8) 0.3691(5) 0.6758(7) 0.0502(15) Uani 1 1 d D . . B9 B 0.7699(7) 0.4416(5) 0.5378(7) 0.0438(13) Uani 1 1 d D . . C1 C 0.2858(7) 0.2613(6) 0.5674(7) 0.0606(18) Uani 1 1 d . . . H1 H 0.2080 0.2480 0.5080 0.073 Uiso 1 1 calc R . . C2 C 0.3357(8) 0.3522(6) 0.6043(7) 0.0622(17) Uani 1 1 d . . . H2 H 0.2992 0.4089 0.5713 0.075 Uiso 1 1 calc R . . C3 C 0.4541(8) 0.3396(7) 0.7031(7) 0.066(2) Uani 1 1 d . . . H3 H 0.5064 0.3871 0.7474 0.079 Uiso 1 1 calc R . . C4 C 0.4760(8) 0.2436(7) 0.7203(7) 0.065(2) Uani 1 1 d . . . H4 H 0.5461 0.2161 0.7777 0.078 Uiso 1 1 calc R . . C5 C 0.3737(9) 0.1950(7) 0.6358(7) 0.0653(19) Uani 1 1 d . . . H5 H 0.3661 0.1303 0.6271 0.078 Uiso 1 1 calc R . . C11 C 0.3143(6) 0.3046(4) 0.1753(5) 0.0363(10) Uani 1 1 d . . . C12 C 0.2429(6) 0.3775(4) 0.2354(5) 0.0413(11) Uani 1 1 d . . . H12 H 0.2599 0.3902 0.3285 0.050 Uiso 1 1 calc R . . C13 C 0.1464(7) 0.4313(4) 0.1573(6) 0.0497(13) Uani 1 1 d . . . H13 H 0.0984 0.4796 0.1985 0.060 Uiso 1 1 calc R . . C14 C 0.1210(6) 0.4138(4) 0.0185(6) 0.0498(13) Uani 1 1 d . . . H14 H 0.0562 0.4501 -0.0334 0.060 Uiso 1 1 calc R . . C15 C 0.1911(7) 0.3436(5) -0.0415(6) 0.0533(14) Uani 1 1 d . . . H15 H 0.1735 0.3316 -0.1347 0.064 Uiso 1 1 calc R . . C16 C 0.2886(8) 0.2894(4) 0.0344(6) 0.0475(14) Uani 1 1 d . . . H16 H 0.3375 0.2424 -0.0088 0.057 Uiso 1 1 calc R . . C21 C 0.5647(6) 0.1982(4) 0.1621(5) 0.0393(11) Uani 1 1 d . . . C22 C 0.6307(7) 0.2716(4) 0.0968(6) 0.0454(12) Uani 1 1 d . . . H22 H 0.5987 0.3326 0.1073 0.055 Uiso 1 1 calc R . . C23 C 0.7437(8) 0.2544(6) 0.0161(8) 0.0601(17) Uani 1 1 d . . . H23 H 0.7893 0.3042 -0.0240 0.072 Uiso 1 1 calc R . . C24 C 0.7880(8) 0.1650(6) -0.0046(8) 0.0680(19) Uani 1 1 d . . . H24 H 0.8623 0.1538 -0.0604 0.082 Uiso 1 1 calc R . . C25 C 0.7235(9) 0.0919(6) 0.0565(9) 0.069(2) Uani 1 1 d . . . H25 H 0.7539 0.0309 0.0423 0.083 Uiso 1 1 calc R . . C26 C 0.6115(7) 0.1088(5) 0.1408(7) 0.0527(14) Uani 1 1 d . . . H26 H 0.5684 0.0587 0.1827 0.063 Uiso 1 1 calc R . . C31 C 0.3239(6) 0.1199(4) 0.2913(5) 0.0379(10) Uani 1 1 d . . . C32 C 0.3795(7) 0.0463(4) 0.3699(7) 0.0511(14) Uani 1 1 d . . . H32 H 0.4707 0.0510 0.4101 0.061 Uiso 1 1 calc R . . C33 C 0.3015(9) -0.0345(5) 0.3896(7) 0.0639(18) Uani 1 1 d . . . H33 H 0.3405 -0.0835 0.4421 0.077 Uiso 1 1 calc R . . C34 C 0.1690(10) -0.0413(5) 0.3322(9) 0.073(2) Uani 1 1 d . . . H34 H 0.1159 -0.0951 0.3453 0.087 Uiso 1 1 calc R . . C35 C 0.1134(8) 0.0300(6) 0.2558(10) 0.077(2) Uani 1 1 d . . . H35 H 0.0222 0.0240 0.2162 0.093 Uiso 1 1 calc R . . C36 C 0.1872(7) 0.1115(5) 0.2342(7) 0.0549(14) Uani 1 1 d . . . H36 H 0.1458 0.1599 0.1822 0.066 Uiso 1 1 calc R . . H1B H 0.850(7) 0.416(4) 0.288(6) 0.050 Uiso 1 1 d D . . H12B H 0.794(7) 0.299(3) 0.308(4) 0.050 Uiso 1 1 d D . . H2B H 0.932(6) 0.220(4) 0.357(7) 0.050 Uiso 1 1 d D . . H3B H 1.020(4) 0.377(4) 0.522(7) 0.050 Uiso 1 1 d D . . H7B H 0.928(7) 0.203(4) 0.659(7) 0.050 Uiso 1 1 d D . . H78B H 0.792(7) 0.293(3) 0.709(6) 0.050 Uiso 1 1 d D . . H8B H 0.911(6) 0.397(4) 0.754(5) 0.050 Uiso 1 1 d D . . H89B H 0.730(5) 0.419(4) 0.655(4) 0.050 Uiso 1 1 d D . . H9B H 0.798(7) 0.515(3) 0.535(7) 0.050 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru5 0.02749(17) 0.04196(19) 0.02900(16) -0.00051(19) 0.00132(11) -0.00082(19) P1 0.0325(7) 0.0337(6) 0.0317(6) -0.0010(4) 0.0001(5) 0.0011(5) S4 0.0376(6) 0.0370(6) 0.0427(6) 0.0042(5) -0.0015(5) 0.0027(5) S6 0.0382(7) 0.0345(6) 0.0524(7) 0.0036(5) -0.0014(6) 0.0027(5) B1 0.037(3) 0.049(3) 0.043(3) 0.002(2) 0.005(2) -0.003(3) B2 0.032(3) 0.051(3) 0.050(3) -0.002(3) 0.003(3) 0.007(3) B3 0.027(3) 0.053(3) 0.049(3) 0.005(3) -0.004(2) -0.005(2) B7 0.038(3) 0.057(3) 0.047(3) 0.010(3) -0.006(3) -0.001(3) B8 0.044(3) 0.064(4) 0.042(3) -0.002(3) -0.010(3) -0.008(3) B9 0.040(3) 0.044(3) 0.046(3) 0.000(2) -0.007(3) -0.005(3) C1 0.027(3) 0.113(6) 0.043(3) -0.001(3) 0.008(2) -0.009(3) C2 0.055(4) 0.076(4) 0.058(4) -0.010(3) 0.024(3) 0.006(3) C3 0.052(4) 0.104(6) 0.044(3) -0.026(4) 0.015(3) -0.012(4) C4 0.044(4) 0.119(7) 0.033(3) 0.007(3) 0.006(3) 0.002(4) C5 0.065(4) 0.085(5) 0.047(3) 0.010(3) 0.017(3) -0.018(4) C11 0.036(2) 0.040(2) 0.033(2) -0.0011(19) -0.0011(19) 0.001(2) C12 0.044(3) 0.042(3) 0.038(2) -0.001(2) 0.003(2) 0.007(2) C13 0.048(3) 0.053(3) 0.048(3) 0.002(2) 0.009(3) 0.018(3) C14 0.043(3) 0.061(3) 0.045(3) 0.009(2) -0.007(2) 0.013(3) C15 0.056(3) 0.067(4) 0.036(2) -0.001(3) -0.005(2) 0.014(3) C16 0.055(4) 0.052(3) 0.035(3) -0.007(2) 0.000(3) 0.012(3) C21 0.038(3) 0.045(3) 0.035(2) -0.004(2) -0.002(2) 0.002(2) C22 0.050(3) 0.051(3) 0.035(3) -0.004(2) 0.007(2) 0.002(2) C23 0.055(4) 0.083(4) 0.043(4) -0.003(3) 0.011(3) -0.008(4) C24 0.048(4) 0.101(6) 0.057(4) -0.015(4) 0.016(3) 0.009(4) C25 0.060(4) 0.061(4) 0.089(5) -0.019(4) 0.015(4) 0.019(3) C26 0.045(3) 0.049(3) 0.064(4) -0.006(3) 0.007(3) 0.007(3) C31 0.037(3) 0.041(2) 0.036(2) -0.0052(19) 0.003(2) -0.003(2) C32 0.056(4) 0.039(3) 0.058(3) 0.001(2) 0.001(3) -0.006(3) C33 0.077(5) 0.050(3) 0.065(4) 0.011(3) 0.009(4) -0.009(3) C34 0.079(5) 0.056(4) 0.086(5) 0.002(4) 0.025(4) -0.026(4) C35 0.046(4) 0.079(5) 0.107(6) -0.001(5) 0.004(4) -0.021(4) C36 0.039(3) 0.060(3) 0.065(4) 0.003(3) -0.003(3) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru5 C5 2.183(7) . ? Ru5 C1 2.185(6) . ? Ru5 C2 2.190(6) . ? Ru5 C4 2.227(6) . ? Ru5 C3 2.238(6) . ? Ru5 P1 2.3016(13) . ? Ru5 S6 2.3945(15) . ? Ru5 S4 2.3977(14) . ? P1 C11 1.829(5) . ? P1 C31 1.836(5) . ? P1 C21 1.839(6) . ? S4 B9 1.899(6) . ? S4 B1 1.919(7) . ? S6 B7 1.897(7) . ? S6 B2 1.908(7) . ? B1 B3 1.779(9) . ? B1 B2 1.795(9) . ? B1 B9 1.968(10) . ? B1 H1B 1.08(4) . ? B1 H12B 1.22(4) . ? B2 B3 1.800(9) . ? B2 B7 1.969(10) . ? B2 H12B 1.26(4) . ? B2 H2B 1.09(4) . ? B3 B8 1.732(10) . ? B3 B9 1.822(9) . ? B3 B7 1.825(10) . ? B3 H3B 1.10(4) . ? B7 B8 1.788(11) . ? B7 H7B 1.08(4) . ? B7 H78B 1.27(4) . ? B8 B9 1.782(9) . ? B8 H78B 1.22(4) . ? B8 H8B 1.08(4) . ? B8 H89B 1.24(4) . ? B9 H89B 1.26(4) . ? B9 H9B 1.08(4) . ? C1 C5 1.403(12) . ? C1 C2 1.420(11) . ? C1 H1 0.93 . ? C2 C3 1.446(11) . ? C2 H2 0.93 . ? C3 C4 1.394(13) . ? C3 H3 0.93 . ? C4 C5 1.416(11) . ? C4 H4 0.93 . ? C5 H5 0.93 . ? C11 C12 1.391(7) . ? C11 C16 1.398(8) . ? C12 C13 1.387(8) . ? C12 H12 0.93 . ? C13 C14 1.382(8) . ? C13 H13 0.93 . ? C14 C15 1.356(9) . ? C14 H14 0.93 . ? C15 C16 1.385(9) . ? C15 H15 0.93 . ? C16 H16 0.93 . ? C21 C26 1.372(8) . ? C21 C22 1.394(9) . ? C22 C23 1.389(10) . ? C22 H22 0.93 . ? C23 C24 1.363(12) . ? C23 H23 0.93 . ? C24 C25 1.365(12) . ? C24 H24 0.93 . ? C25 C26 1.403(10) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C31 C36 1.385(8) . ? C31 C32 1.386(8) . ? C32 C33 1.389(9) . ? C32 H32 0.93 . ? C33 C34 1.348(12) . ? C33 H33 0.93 . ? C34 C35 1.351(12) . ? C34 H34 0.93 . ? C35 C36 1.379(10) . ? C35 H35 0.93 . ? C36 H36 0.93 . ? 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 C5 Ru5 C1 37.5(3) . . ? C5 Ru5 C2 63.2(4) . . ? C1 Ru5 C2 37.9(3) . . ? C5 Ru5 C4 37.4(3) . . ? C1 Ru5 C4 62.3(3) . . ? C2 Ru5 C4 62.6(3) . . ? C5 Ru5 C3 62.2(3) . . ? C1 Ru5 C3 62.7(3) . . ? C2 Ru5 C3 38.1(3) . . ? C4 Ru5 C3 36.4(3) . . ? C5 Ru5 P1 104.6(2) . . ? C1 Ru5 P1 91.18(19) . . ? C2 Ru5 P1 113.8(2) . . ? C4 Ru5 P1 141.4(2) . . ? C3 Ru5 P1 151.4(2) . . ? C5 Ru5 S6 101.9(3) . . ? C1 Ru5 S6 138.1(2) . . ? C2 Ru5 S6 152.2(2) . . ? C4 Ru5 S6 91.0(2) . . ? C3 Ru5 S6 114.8(2) . . ? P1 Ru5 S6 92.09(5) . . ? C5 Ru5 S4 158.2(2) . . ? C1 Ru5 S4 130.1(2) . . ? C2 Ru5 S4 97.3(2) . . ? C4 Ru5 S4 126.4(2) . . ? C3 Ru5 S4 96.6(2) . . ? P1 Ru5 S4 91.88(5) . . ? S6 Ru5 S4 91.46(5) . . ? C11 P1 C31 103.0(2) . . ? C11 P1 C21 100.9(2) . . ? C31 P1 C21 104.1(2) . . ? C11 P1 Ru5 118.03(17) . . ? C31 P1 Ru5 110.08(17) . . ? C21 P1 Ru5 118.80(18) . . ? B9 S4 B1 62.0(3) . . ? B9 S4 Ru5 107.3(2) . . ? B1 S4 Ru5 108.1(2) . . ? B7 S6 B2 62.3(3) . . ? B7 S6 Ru5 107.5(2) . . ? B2 S6 Ru5 109.0(2) . . ? B3 B1 B2 60.5(4) . . ? B3 B1 S4 109.4(4) . . ? B2 B1 S4 115.8(4) . . ? B3 B1 B9 57.9(3) . . ? B2 B1 B9 106.8(4) . . ? S4 B1 B9 58.5(3) . . ? B3 B1 H1B 115(4) . . ? B2 B1 H1B 124(3) . . ? S4 B1 H1B 117(4) . . ? B9 B1 H1B 116(3) . . ? B3 B1 H12B 104.3(19) . . ? B2 B1 H12B 44.3(17) . . ? S4 B1 H12B 109(3) . . ? B9 B1 H12B 144(3) . . ? H1B B1 H12B 100(4) . . ? B1 B2 B3 59.3(4) . . ? B1 B2 S6 114.8(4) . . ? B3 B2 S6 108.8(4) . . ? B1 B2 B7 105.5(5) . . ? B3 B2 B7 57.7(4) . . ? S6 B2 B7 58.6(3) . . ? B1 B2 H12B 42.8(17) . . ? B3 B2 H12B 101.6(18) . . ? S6 B2 H12B 109(3) . . ? B7 B2 H12B 142(3) . . ? B1 B2 H2B 122(4) . . ? B3 B2 H2B 118(4) . . ? S6 B2 H2B 118(3) . . ? B7 B2 H2B 120(4) . . ? H12B B2 H2B 98(5) . . ? B8 B3 B1 119.3(5) . . ? B8 B3 B2 119.2(5) . . ? B1 B3 B2 60.2(3) . . ? B8 B3 B9 60.1(4) . . ? B1 B3 B9 66.2(4) . . ? B2 B3 B9 113.2(4) . . ? B8 B3 B7 60.3(4) . . ? B1 B3 B7 112.6(4) . . ? B2 B3 B7 65.8(4) . . ? B9 B3 B7 105.0(5) . . ? B8 B3 H3B 112(4) . . ? B1 B3 H3B 119(3) . . ? B2 B3 H3B 119(3) . . ? B9 B3 H3B 120(3) . . ? B7 B3 H3B 121(3) . . ? B8 B7 B3 57.3(4) . . ? B8 B7 S6 125.5(4) . . ? B3 B7 S6 108.3(4) . . ? B8 B7 B2 108.3(5) . . ? B3 B7 B2 56.5(4) . . ? S6 B7 B2 59.1(3) . . ? B8 B7 H7B 122(4) . . ? B3 B7 H7B 122(4) . . ? S6 B7 H7B 110(4) . . ? B2 B7 H7B 114(4) . . ? B8 B7 H78B 42.8(17) . . ? B3 B7 H78B 99.4(18) . . ? S6 B7 H78B 108(3) . . ? B2 B7 H78B 138(3) . . ? H7B B7 H78B 107(5) . . ? B3 B8 B9 62.4(4) . . ? B3 B8 B7 62.4(4) . . ? B9 B8 B7 108.3(5) . . ? B3 B8 H78B 107.0(19) . . ? B9 B8 H78B 127(4) . . ? B7 B8 H78B 45.3(18) . . ? B3 B8 H8B 113(4) . . ? B9 B8 H8B 120(4) . . ? B7 B8 H8B 121(4) . . ? H78B B8 H8B 111(5) . . ? B3 B8 H89B 106.2(18) . . ? B9 B8 H89B 45.1(17) . . ? B7 B8 H89B 124(3) . . ? H78B B8 H89B 106(4) . . ? H8B B8 H89B 113(4) . . ? B8 B9 B3 57.4(4) . . ? B8 B9 S4 125.7(4) . . ? B3 B9 S4 108.4(4) . . ? B8 B9 B1 107.7(5) . . ? B3 B9 B1 55.8(3) . . ? S4 B9 B1 59.5(3) . . ? B8 B9 H89B 44.2(17) . . ? B3 B9 H89B 100.4(18) . . ? S4 B9 H89B 105(3) . . ? B1 B9 H89B 136(3) . . ? B8 B9 H9B 120(4) . . ? B3 B9 H9B 118(4) . . ? S4 B9 H9B 112(4) . . ? B1 B9 H9B 113(3) . . ? H89B B9 H9B 111(4) . . ? C5 C1 C2 108.5(7) . . ? C5 C1 Ru5 71.2(4) . . ? C2 C1 Ru5 71.3(4) . . ? C5 C1 H1 125.8 . . ? C2 C1 H1 125.8 . . ? Ru5 C1 H1 123.4 . . ? C1 C2 C3 106.8(7) . . ? C1 C2 Ru5 70.9(4) . . ? C3 C2 Ru5 72.8(4) . . ? C1 C2 H2 126.6 . . ? C3 C2 H2 126.6 . . ? Ru5 C2 H2 121.6 . . ? C4 C3 C2 107.8(7) . . ? C4 C3 Ru5 71.4(4) . . ? C2 C3 Ru5 69.1(3) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? Ru5 C3 H3 125.0 . . ? C3 C4 C5 108.7(7) . . ? C3 C4 Ru5 72.2(4) . . ? C5 C4 Ru5 69.6(4) . . ? C3 C4 H4 125.7 . . ? C5 C4 H4 125.7 . . ? Ru5 C4 H4 124.1 . . ? C1 C5 C4 108.2(8) . . ? C1 C5 Ru5 71.3(4) . . ? C4 C5 Ru5 73.0(4) . . ? C1 C5 H5 125.9 . . ? C4 C5 H5 125.9 . . ? Ru5 C5 H5 121.5 . . ? C12 C11 C16 118.1(5) . . ? C12 C11 P1 119.9(4) . . ? C16 C11 P1 121.9(4) . . ? C13 C12 C11 120.3(5) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 120.5(5) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 119.7(5) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.7(5) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C11 120.6(5) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? C26 C21 C22 118.2(6) . . ? C26 C21 P1 123.6(5) . . ? C22 C21 P1 118.1(4) . . ? C23 C22 C21 120.6(6) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 120.3(7) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 120.1(6) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 119.9(6) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 120.8(6) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C36 C31 C32 118.2(5) . . ? C36 C31 P1 123.4(5) . . ? C32 C31 P1 118.1(4) . . ? C31 C32 C33 121.2(7) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C34 C33 C32 119.6(7) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 119.8(7) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C36 122.4(7) . . ? C34 C35 H35 118.8 . . ? C36 C35 H35 118.8 . . ? C35 C36 C31 118.8(6) . . ? C35 C36 H36 120.6 . . ? C31 C36 H36 120.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 Ru5 P1 C11 105.0(3) . . . . ? C1 Ru5 P1 C11 69.7(3) . . . . ? C2 Ru5 P1 C11 38.3(3) . . . . ? C4 Ru5 P1 C11 113.6(4) . . . . ? C3 Ru5 P1 C11 47.0(6) . . . . ? S6 Ru5 P1 C11 -152.1(2) . . . . ? S4 Ru5 P1 C11 -60.6(2) . . . . ? C5 Ru5 P1 C31 -12.7(3) . . . . ? C1 Ru5 P1 C31 -48.1(3) . . . . ? C2 Ru5 P1 C31 -79.5(3) . . . . ? C4 Ru5 P1 C31 -4.1(4) . . . . ? C3 Ru5 P1 C31 -70.8(6) . . . . ? S6 Ru5 P1 C31 90.19(19) . . . . ? S4 Ru5 P1 C31 -178.28(19) . . . . ? C5 Ru5 P1 C21 -132.5(3) . . . . ? C1 Ru5 P1 C21 -167.9(3) . . . . ? C2 Ru5 P1 C21 160.7(3) . . . . ? C4 Ru5 P1 C21 -124.0(4) . . . . ? C3 Ru5 P1 C21 169.4(6) . . . . ? S6 Ru5 P1 C21 -29.7(2) . . . . ? S4 Ru5 P1 C21 61.9(2) . . . . ? C5 Ru5 S4 B9 70.6(7) . . . . ? C1 Ru5 S4 B9 117.1(3) . . . . ? C2 Ru5 S4 B9 95.9(3) . . . . ? C4 Ru5 S4 B9 34.7(4) . . . . ? C3 Ru5 S4 B9 57.5(3) . . . . ? P1 Ru5 S4 B9 -149.8(2) . . . . ? S6 Ru5 S4 B9 -57.6(2) . . . . ? C5 Ru5 S4 B1 136.0(6) . . . . ? C1 Ru5 S4 B1 -177.4(3) . . . . ? C2 Ru5 S4 B1 161.4(3) . . . . ? C4 Ru5 S4 B1 100.2(3) . . . . ? C3 Ru5 S4 B1 123.0(3) . . . . ? P1 Ru5 S4 B1 -84.3(2) . . . . ? S6 Ru5 S4 B1 7.8(2) . . . . ? C5 Ru5 S6 B7 -104.9(3) . . . . ? C1 Ru5 S6 B7 -116.2(4) . . . . ? C2 Ru5 S6 B7 -51.0(5) . . . . ? C4 Ru5 S6 B7 -68.7(3) . . . . ? C3 Ru5 S6 B7 -40.2(3) . . . . ? P1 Ru5 S6 B7 149.7(2) . . . . ? S4 Ru5 S6 B7 57.8(2) . . . . ? C5 Ru5 S6 B2 -170.9(3) . . . . ? C1 Ru5 S6 B2 177.8(4) . . . . ? C2 Ru5 S6 B2 -117.0(5) . . . . ? C4 Ru5 S6 B2 -134.7(3) . . . . ? C3 Ru5 S6 B2 -106.2(3) . . . . ? P1 Ru5 S6 B2 83.7(2) . . . . ? S4 Ru5 S6 B2 -8.2(2) . . . . ? B9 S4 B1 B3 28.9(4) . . . . ? Ru5 S4 B1 B3 -71.5(4) . . . . ? B9 S4 B1 B2 94.6(5) . . . . ? Ru5 S4 B1 B2 -5.7(5) . . . . ? Ru5 S4 B1 B9 -100.4(3) . . . . ? S4 B1 B2 B3 -98.6(5) . . . . ? B9 B1 B2 B3 -36.0(4) . . . . ? B3 B1 B2 S6 98.0(5) . . . . ? S4 B1 B2 S6 -0.6(6) . . . . ? B9 B1 B2 S6 62.0(5) . . . . ? B3 B1 B2 B7 35.9(4) . . . . ? S4 B1 B2 B7 -62.7(5) . . . . ? B9 B1 B2 B7 -0.1(5) . . . . ? B7 S6 B2 B1 -93.6(5) . . . . ? Ru5 S6 B2 B1 6.6(5) . . . . ? B7 S6 B2 B3 -29.5(4) . . . . ? Ru5 S6 B2 B3 70.8(4) . . . . ? Ru5 S6 B2 B7 100.3(3) . . . . ? B2 B1 B3 B8 -108.9(6) . . . . ? S4 B1 B3 B8 0.4(6) . . . . ? B9 B1 B3 B8 29.5(5) . . . . ? S4 B1 B3 B2 109.3(4) . . . . ? B9 B1 B3 B2 138.4(5) . . . . ? B2 B1 B3 B9 -138.4(5) . . . . ? S4 B1 B3 B9 -29.1(4) . . . . ? B2 B1 B3 B7 -41.3(5) . . . . ? S4 B1 B3 B7 68.0(6) . . . . ? B9 B1 B3 B7 97.0(5) . . . . ? B1 B2 B3 B8 109.0(6) . . . . ? S6 B2 B3 B8 0.7(6) . . . . ? B7 B2 B3 B8 -29.0(5) . . . . ? S6 B2 B3 B1 -108.2(4) . . . . ? B7 B2 B3 B1 -138.0(5) . . . . ? B1 B2 B3 B9 41.4(5) . . . . ? S6 B2 B3 B9 -66.9(5) . . . . ? B7 B2 B3 B9 -96.6(5) . . . . ? B1 B2 B3 B7 138.0(5) . . . . ? S6 B2 B3 B7 29.8(4) . . . . ? B1 B3 B7 B8 -111.8(5) . . . . ? B2 B3 B7 B8 -150.8(5) . . . . ? B9 B3 B7 B8 -41.7(4) . . . . ? B8 B3 B7 S6 120.9(5) . . . . ? B1 B3 B7 S6 9.1(6) . . . . ? B2 B3 B7 S6 -29.9(4) . . . . ? B9 B3 B7 S6 79.2(5) . . . . ? B8 B3 B7 B2 150.8(5) . . . . ? B1 B3 B7 B2 39.0(4) . . . . ? B9 B3 B7 B2 109.1(4) . . . . ? B2 S6 B7 B8 91.3(6) . . . . ? Ru5 S6 B7 B8 -11.4(6) . . . . ? B2 S6 B7 B3 29.0(4) . . . . ? Ru5 S6 B7 B3 -73.8(4) . . . . ? Ru5 S6 B7 B2 -102.7(3) . . . . ? B1 B2 B7 B8 -11.0(6) . . . . ? B3 B2 B7 B8 25.6(4) . . . . ? S6 B2 B7 B8 -120.9(5) . . . . ? B1 B2 B7 B3 -36.6(4) . . . . ? S6 B2 B7 B3 -146.6(4) . . . . ? B1 B2 B7 S6 109.9(4) . . . . ? B3 B2 B7 S6 146.6(4) . . . . ? B1 B3 B8 B9 -31.3(5) . . . . ? B2 B3 B8 B9 -101.5(5) . . . . ? B7 B3 B8 B9 -132.1(4) . . . . ? B1 B3 B8 B7 100.8(5) . . . . ? B2 B3 B8 B7 30.7(5) . . . . ? B9 B3 B8 B7 132.1(4) . . . . ? S6 B7 B8 B3 -90.0(5) . . . . ? B2 B7 B8 B3 -25.4(4) . . . . ? B3 B7 B8 B9 43.8(4) . . . . ? S6 B7 B8 B9 -46.2(7) . . . . ? B2 B7 B8 B9 18.4(6) . . . . ? B7 B8 B9 B3 -43.8(5) . . . . ? B3 B8 B9 S4 90.2(5) . . . . ? B7 B8 B9 S4 46.4(7) . . . . ? B3 B8 B9 B1 25.5(4) . . . . ? B7 B8 B9 B1 -18.3(6) . . . . ? B1 B3 B9 B8 150.3(5) . . . . ? B2 B3 B9 B8 111.5(5) . . . . ? B7 B3 B9 B8 41.8(4) . . . . ? B8 B3 B9 S4 -121.1(5) . . . . ? B1 B3 B9 S4 29.2(4) . . . . ? B2 B3 B9 S4 -9.6(6) . . . . ? B7 B3 B9 S4 -79.3(5) . . . . ? B8 B3 B9 B1 -150.3(5) . . . . ? B2 B3 B9 B1 -38.8(4) . . . . ? B7 B3 B9 B1 -108.5(5) . . . . ? B1 S4 B9 B8 -90.6(6) . . . . ? Ru5 S4 B9 B8 11.1(6) . . . . ? B1 S4 B9 B3 -28.0(4) . . . . ? Ru5 S4 B9 B3 73.8(4) . . . . ? Ru5 S4 B9 B1 101.7(3) . . . . ? B3 B1 B9 B8 -26.0(4) . . . . ? B2 B1 B9 B8 11.2(6) . . . . ? S4 B1 B9 B8 121.5(5) . . . . ? B2 B1 B9 B3 37.1(4) . . . . ? S4 B1 B9 B3 147.5(4) . . . . ? B3 B1 B9 S4 -147.5(4) . . . . ? B2 B1 B9 S4 -110.3(4) . . . . ? C2 Ru5 C1 C5 -118.0(7) . . . . ? C4 Ru5 C1 C5 -37.9(5) . . . . ? C3 Ru5 C1 C5 -79.1(5) . . . . ? P1 Ru5 C1 C5 112.9(5) . . . . ? S6 Ru5 C1 C5 18.4(6) . . . . ? S4 Ru5 C1 C5 -153.7(4) . . . . ? C5 Ru5 C1 C2 118.0(7) . . . . ? C4 Ru5 C1 C2 80.1(5) . . . . ? C3 Ru5 C1 C2 38.9(5) . . . . ? P1 Ru5 C1 C2 -129.1(4) . . . . ? S6 Ru5 C1 C2 136.4(4) . . . . ? S4 Ru5 C1 C2 -35.7(5) . . . . ? C5 C1 C2 C3 -2.6(7) . . . . ? Ru5 C1 C2 C3 -64.4(4) . . . . ? C5 C1 C2 Ru5 61.8(5) . . . . ? C5 Ru5 C2 C1 -37.0(4) . . . . ? C4 Ru5 C2 C1 -79.3(5) . . . . ? C3 Ru5 C2 C1 -115.3(7) . . . . ? P1 Ru5 C2 C1 58.0(5) . . . . ? S6 Ru5 C2 C1 -99.4(6) . . . . ? S4 Ru5 C2 C1 153.3(4) . . . . ? C5 Ru5 C2 C3 78.3(5) . . . . ? C1 Ru5 C2 C3 115.3(7) . . . . ? C4 Ru5 C2 C3 36.1(5) . . . . ? P1 Ru5 C2 C3 173.3(4) . . . . ? S6 Ru5 C2 C3 15.9(8) . . . . ? S4 Ru5 C2 C3 -91.4(5) . . . . ? C1 C2 C3 C4 1.9(7) . . . . ? Ru5 C2 C3 C4 -61.2(5) . . . . ? C1 C2 C3 Ru5 63.1(4) . . . . ? C5 Ru5 C3 C4 37.1(5) . . . . ? C1 Ru5 C3 C4 79.6(5) . . . . ? C2 Ru5 C3 C4 118.3(7) . . . . ? P1 Ru5 C3 C4 105.3(6) . . . . ? S6 Ru5 C3 C4 -53.6(5) . . . . ? S4 Ru5 C3 C4 -148.3(4) . . . . ? C5 Ru5 C3 C2 -81.1(5) . . . . ? C1 Ru5 C3 C2 -38.7(5) . . . . ? C4 Ru5 C3 C2 -118.3(7) . . . . ? P1 Ru5 C3 C2 -12.9(8) . . . . ? S6 Ru5 C3 C2 -171.9(4) . . . . ? S4 Ru5 C3 C2 93.4(5) . . . . ? C2 C3 C4 C5 -0.5(7) . . . . ? Ru5 C3 C4 C5 -60.3(5) . . . . ? C2 C3 C4 Ru5 59.8(4) . . . . ? C5 Ru5 C4 C3 -118.6(7) . . . . ? C1 Ru5 C4 C3 -80.7(5) . . . . ? C2 Ru5 C4 C3 -37.7(4) . . . . ? P1 Ru5 C4 C3 -132.3(4) . . . . ? S6 Ru5 C4 C3 133.0(4) . . . . ? S4 Ru5 C4 C3 40.5(5) . . . . ? C1 Ru5 C4 C5 37.9(5) . . . . ? C2 Ru5 C4 C5 80.8(6) . . . . ? C3 Ru5 C4 C5 118.6(7) . . . . ? P1 Ru5 C4 C5 -13.7(7) . . . . ? S6 Ru5 C4 C5 -108.4(5) . . . . ? S4 Ru5 C4 C5 159.0(5) . . . . ? C2 C1 C5 C4 2.3(8) . . . . ? Ru5 C1 C5 C4 64.1(5) . . . . ? C2 C1 C5 Ru5 -61.8(5) . . . . ? C3 C4 C5 C1 -1.1(8) . . . . ? Ru5 C4 C5 C1 -63.1(5) . . . . ? C3 C4 C5 Ru5 62.0(5) . . . . ? C2 Ru5 C5 C1 37.4(5) . . . . ? C4 Ru5 C5 C1 116.6(7) . . . . ? C3 Ru5 C5 C1 80.5(5) . . . . ? P1 Ru5 C5 C1 -72.2(5) . . . . ? S6 Ru5 C5 C1 -167.6(4) . . . . ? S4 Ru5 C5 C1 65.8(8) . . . . ? C1 Ru5 C5 C4 -116.6(7) . . . . ? C2 Ru5 C5 C4 -79.2(6) . . . . ? C3 Ru5 C5 C4 -36.1(5) . . . . ? P1 Ru5 C5 C4 171.2(5) . . . . ? S6 Ru5 C5 C4 75.8(5) . . . . ? S4 Ru5 C5 C4 -50.8(9) . . . . ? C31 P1 C11 C12 104.7(5) . . . . ? C21 P1 C11 C12 -147.9(5) . . . . ? Ru5 P1 C11 C12 -16.8(5) . . . . ? C31 P1 C11 C16 -71.4(5) . . . . ? C21 P1 C11 C16 36.0(6) . . . . ? Ru5 P1 C11 C16 167.1(4) . . . . ? C16 C11 C12 C13 1.7(9) . . . . ? P1 C11 C12 C13 -174.5(5) . . . . ? C11 C12 C13 C14 -0.6(10) . . . . ? C12 C13 C14 C15 -0.1(10) . . . . ? C13 C14 C15 C16 -0.4(10) . . . . ? C14 C15 C16 C11 1.6(10) . . . . ? C12 C11 C16 C15 -2.2(9) . . . . ? P1 C11 C16 C15 173.9(5) . . . . ? C11 P1 C21 C26 -132.8(5) . . . . ? C31 P1 C21 C26 -26.3(6) . . . . ? Ru5 P1 C21 C26 96.5(5) . . . . ? C11 P1 C21 C22 52.0(5) . . . . ? C31 P1 C21 C22 158.5(4) . . . . ? Ru5 P1 C21 C22 -78.7(5) . . . . ? C26 C21 C22 C23 -2.1(9) . . . . ? P1 C21 C22 C23 173.4(5) . . . . ? C21 C22 C23 C24 2.6(11) . . . . ? C22 C23 C24 C25 -1.5(11) . . . . ? C23 C24 C25 C26 0.0(12) . . . . ? C22 C21 C26 C25 0.6(10) . . . . ? P1 C21 C26 C25 -174.6(6) . . . . ? C24 C25 C26 C21 0.5(12) . . . . ? C11 P1 C31 C36 -4.1(5) . . . . ? C21 P1 C31 C36 -109.0(5) . . . . ? Ru5 P1 C31 C36 122.6(5) . . . . ? C11 P1 C31 C32 -178.1(5) . . . . ? C21 P1 C31 C32 77.0(5) . . . . ? Ru5 P1 C31 C32 -51.4(5) . . . . ? C36 C31 C32 C33 0.9(9) . . . . ? P1 C31 C32 C33 175.2(5) . . . . ? C31 C32 C33 C34 -0.4(11) . . . . ? C32 C33 C34 C35 0.3(12) . . . . ? C33 C34 C35 C36 -0.5(13) . . . . ? C34 C35 C36 C31 1.0(13) . . . . ? C32 C31 C36 C35 -1.1(10) . . . . ? P1 C31 C36 C35 -175.1(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.145 _refine_diff_density_min -1.173 _refine_diff_density_rms 0.079 #========================================================================= # END of CIF for Compound 1 #========================================================================= data_compd-2 _database_code_depnum_ccdc_archive 'CCDC 264503' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H44 B6 P2 Ru S2' _chemical_formula_sum 'C41 H44 B6 P2 Ru S2' _chemical_formula_weight 828.75 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' B B 0.0013 0.0007 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.0113(9) _cell_length_b 18.7264(16) _cell_length_c 19.840(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.546(10) _cell_angle_gamma 90.00 _cell_volume 4072.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 294(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.2 _cell_measurement_theta_max 18.3 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 0.596 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.7966 _exptl_absorpt_correction_T_max 0.8187 _exptl_absorpt_process_details 'ABSORB in NRCVAX (Gabe et al., 1989)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(1) _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 'CAD4 diffractometer' _diffrn_measurement_method '\t,/2\t scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 4.3 _diffrn_reflns_number 8839 _diffrn_reflns_av_R_equivalents 0.015 _diffrn_reflns_av_sigmaI/netI 0.0764 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8839 _reflns_number_gt 5438 _reflns_threshold_expression >2\s(I) _computing_data_collection 'DIFRAC (Gabe & White, 1993)' _computing_cell_refinement 'DIFRAC (Gabe & White, 1993)' _computing_data_reduction 'DATRD2 in NRCVAX94 (Gabe, Le Page, Charland, Lee & White, 1989)' _computing_structure_solution 'Patterson heavy-atom method and NRCVAX94' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'NRCVAX94, SHELXL97' #========================================================================= _refine_special_details ; Molecule (I) crystallised in the monoclinic system; space group P2~1~/n from the systematic absences. It became obvious during the structure determination that there was disorder in the structure. In particular two small peaks (approx 1 e %A^-3^) corresponding with other orientations for S atom S2 were visible and labelled as S2A and S2B. Coordinates for these two sites were determined from difference maps and included with a Uiso value of 0.05 \%A^2^ but not refined in subsequent calculations. Occupancy factor refinement using the SUMP control in SHELXL97 led to occupancy values of 0.906(3), 0.051(2) and 0.043(2) for S2, S2A and S2B respectively. It was not possible to locate B atoms corresponding with the disordered low-occupancy S atoms S2A and S2B. All H atoms were visible in difference maps. Those bonded to C were treated as riding atoms (Shelxl AFIX 43) with C-H 0.93\%A. Terminal B-H H atoms were restrained with a DFIX 1.10(4)\%A command; bridging B-H-B H atoms were restrained with a DFIX 1.24(4)\%A command. ; # Refinement Data _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^)+(0.0446P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8839 _refine_ls_number_parameters 499 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.953 _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 0.32830(2) 0.259703(14) 0.025556(13) 0.03237(8) Uani 1 1 d . . . S1 S 0.22125(8) 0.21236(5) -0.07589(4) 0.0398(2) Uani 1 1 d . . . S2 S 0.03502(13) 0.08954(10) -0.18362(8) 0.0908(7) Uani 0.906(3) 1 d P . . S2A S 0.0235 0.1377 -0.2155 0.050 Uiso 0.051(2) 1 d P . . S2B S 0.1332 0.2504 -0.2547 0.050 Uiso 0.043(2) 1 d P . . P1 P 0.22490(8) 0.18427(5) 0.09609(4) 0.0344(2) Uani 1 1 d . . . P2 P 0.19168(8) 0.35512(4) 0.01553(4) 0.0334(2) Uani 1 1 d . . . C1 C 0.4795(3) 0.2990(2) 0.0958(2) 0.0562(11) Uani 1 1 d . . . H1 H 0.4658 0.3180 0.1378 0.067 Uiso 1 1 calc R . . C2 C 0.4798(3) 0.3368(2) 0.0347(2) 0.0550(10) Uani 1 1 d . . . H2 H 0.4681 0.3858 0.0293 0.066 Uiso 1 1 calc R . . C3 C 0.5006(3) 0.2887(2) -0.0168(2) 0.0517(10) Uani 1 1 d . . . H3 H 0.5041 0.2997 -0.0623 0.062 Uiso 1 1 calc R . . C4 C 0.5152(3) 0.2200(2) 0.0128(2) 0.0526(10) Uani 1 1 d . . . H4 H 0.5299 0.1778 -0.0097 0.063 Uiso 1 1 calc R . . C5 C 0.5037(3) 0.2275(2) 0.0818(2) 0.0570(11) Uani 1 1 d . . . H5 H 0.5109 0.1908 0.1135 0.068 Uiso 1 1 calc R . . C11 C 0.0669(3) 0.15073(18) 0.08101(19) 0.0441(9) Uani 1 1 d . . . C12 C 0.0325(3) 0.11930(19) 0.0184(2) 0.0546(10) Uani 1 1 d . . . H12 H 0.0864 0.1197 -0.0149 0.066 Uiso 1 1 calc R . . C13 C -0.0815(4) 0.0874(2) 0.0050(2) 0.0671(12) Uani 1 1 d . . . H13 H -0.1032 0.0664 -0.0370 0.080 Uiso 1 1 calc R . . C14 C -0.1608(4) 0.0869(3) 0.0532(3) 0.0801(15) Uani 1 1 d . . . H14 H -0.2374 0.0661 0.0440 0.096 Uiso 1 1 calc R . . C15 C -0.1292(4) 0.1166(3) 0.1150(3) 0.0813(15) Uani 1 1 d . . . H15 H -0.1843 0.1160 0.1477 0.098 Uiso 1 1 calc R . . C16 C -0.0148(3) 0.1479(2) 0.1297(2) 0.0593(11) Uani 1 1 d . . . H16 H 0.0068 0.1669 0.1725 0.071 Uiso 1 1 calc R . . C21 C 0.2953(3) 0.09519(17) 0.11053(17) 0.0397(8) Uani 1 1 d . . . C22 C 0.3732(4) 0.0676(2) 0.06838(19) 0.0548(10) Uani 1 1 d . . . H22 H 0.3937 0.0943 0.0316 0.066 Uiso 1 1 calc R . . C23 C 0.4225(4) 0.0001(2) 0.0796(2) 0.0805(16) Uani 1 1 d . . . H23 H 0.4765 -0.0178 0.0505 0.097 Uiso 1 1 calc R . . C24 C 0.3932(4) -0.0403(2) 0.1323(2) 0.0711(14) Uani 1 1 d . . . H24 H 0.4267 -0.0855 0.1396 0.085 Uiso 1 1 calc R . . C25 C 0.3146(4) -0.0137(2) 0.1743(2) 0.0771(15) Uani 1 1 d . . . H25 H 0.2943 -0.0409 0.2108 0.093 Uiso 1 1 calc R . . C26 C 0.2642(4) 0.0532(2) 0.1635(2) 0.0636(12) Uani 1 1 d . . . H26 H 0.2087 0.0702 0.1921 0.076 Uiso 1 1 calc R . . C31 C 0.2342(3) 0.22059(17) 0.18212(17) 0.0398(8) Uani 1 1 d . . . C32 C 0.3326(4) 0.2056(2) 0.2293(2) 0.0624(11) Uani 1 1 d . . . H32 H 0.3928 0.1741 0.2182 0.075 Uiso 1 1 calc R . . C33 C 0.3417(5) 0.2373(3) 0.2933(2) 0.0818(14) Uani 1 1 d . . . H33 H 0.4082 0.2272 0.3244 0.098 Uiso 1 1 calc R . . C34 C 0.2531(6) 0.2831(3) 0.3103(2) 0.0847(16) Uani 1 1 d . . . H34 H 0.2587 0.3037 0.3531 0.102 Uiso 1 1 calc R . . C35 C 0.1571(5) 0.2987(2) 0.2647(2) 0.0718(13) Uani 1 1 d . . . H35 H 0.0965 0.3296 0.2765 0.086 Uiso 1 1 calc R . . C36 C 0.1486(4) 0.26871(19) 0.20049(19) 0.0525(10) Uani 1 1 d . . . H36 H 0.0838 0.2813 0.1692 0.063 Uiso 1 1 calc R . . C41 C 0.1643(3) 0.39031(17) -0.07179(17) 0.0390(8) Uani 1 1 d . . . C42 C 0.2628(4) 0.4026(2) -0.1086(2) 0.0615(11) Uani 1 1 d . . . H42 H 0.3412 0.3924 -0.0893 0.074 Uiso 1 1 calc R . . C43 C 0.2465(5) 0.4297(2) -0.1739(2) 0.0767(14) Uani 1 1 d . . . H43 H 0.3136 0.4382 -0.1978 0.092 Uiso 1 1 calc R . . C44 C 0.1311(5) 0.4439(2) -0.2030(2) 0.0741(14) Uani 1 1 d . . . H44 H 0.1198 0.4616 -0.2470 0.089 Uiso 1 1 calc R . . C45 C 0.0332(4) 0.4324(2) -0.1679(2) 0.0705(13) Uani 1 1 d . . . H45 H -0.0451 0.4420 -0.1877 0.085 Uiso 1 1 calc R . . C46 C 0.0502(4) 0.4060(2) -0.10211(19) 0.0534(10) Uani 1 1 d . . . H46 H -0.0173 0.3988 -0.0782 0.064 Uiso 1 1 calc R . . C51 C 0.0360(3) 0.34585(17) 0.03930(17) 0.0355(8) Uani 1 1 d . . . C52 C -0.0373(3) 0.29232(18) 0.00824(19) 0.0445(9) Uani 1 1 d . . . H52 H -0.0080 0.2636 -0.0249 0.053 Uiso 1 1 calc R . . C53 C -0.1535(3) 0.2822(2) 0.0268(2) 0.0558(10) Uani 1 1 d . . . H53 H -0.2027 0.2468 0.0057 0.067 Uiso 1 1 calc R . . C54 C -0.1971(3) 0.3229(2) 0.0754(2) 0.0598(11) Uani 1 1 d . . . H54 H -0.2750 0.3146 0.0880 0.072 Uiso 1 1 calc R . . C55 C -0.1267(3) 0.3767(2) 0.1062(2) 0.0560(11) Uani 1 1 d . . . H55 H -0.1571 0.4048 0.1395 0.067 Uiso 1 1 calc R . . C56 C -0.0102(3) 0.38887(19) 0.08743(18) 0.0440(9) Uani 1 1 d . . . H56 H 0.0367 0.4260 0.1072 0.053 Uiso 1 1 calc R . . C61 C 0.2471(3) 0.43505(17) 0.06306(18) 0.0380(8) Uani 1 1 d . . . C62 C 0.2932(3) 0.42800(19) 0.13041(19) 0.0477(9) Uani 1 1 d . . . H62 H 0.2931 0.3834 0.1510 0.057 Uiso 1 1 calc R . . C63 C 0.3395(4) 0.4864(2) 0.1676(2) 0.0566(11) Uani 1 1 d . . . H63 H 0.3717 0.4807 0.2123 0.068 Uiso 1 1 calc R . . C64 C 0.3375(4) 0.5526(2) 0.1381(2) 0.0616(11) Uani 1 1 d . . . H64 H 0.3681 0.5920 0.1629 0.074 Uiso 1 1 calc R . . C65 C 0.2905(4) 0.5608(2) 0.0723(2) 0.0627(12) Uani 1 1 d . . . H65 H 0.2892 0.6058 0.0525 0.075 Uiso 1 1 calc R . . C66 C 0.2447(3) 0.50247(19) 0.0345(2) 0.0500(10) Uani 1 1 d . . . H66 H 0.2122 0.5088 -0.0102 0.060 Uiso 1 1 calc R . . B3 B 0.1356(6) 0.1287(3) -0.2435(3) 0.0767(17) Uani 1 1 d D . . B4 B 0.2111(7) 0.2140(3) -0.2391(3) 0.0798(18) Uani 1 1 d D . . B5 B 0.2926(5) 0.2267(3) -0.1571(2) 0.0595(13) Uani 1 1 d D . . B6 B 0.2947(4) 0.1314(2) -0.1116(2) 0.0477(11) Uani 1 1 d D . . B7 B 0.2018(5) 0.0714(3) -0.1667(3) 0.0665(15) Uani 1 1 d D . . B8 B 0.2879(4) 0.1411(3) -0.2017(2) 0.0514(11) Uani 1 1 d D . . H3B H 0.125(3) 0.1111(17) -0.2943(14) 0.050 Uiso 1 1 d D . . H4B H 0.241(3) 0.2367(17) -0.2845(15) 0.050 Uiso 1 1 d D . . H5B H 0.378(3) 0.2590(16) -0.1585(17) 0.050 Uiso 1 1 d D . . H6B H 0.386(2) 0.1157(17) -0.0893(16) 0.050 Uiso 1 1 d D . . H7B H 0.240(3) 0.0222(15) -0.1787(17) 0.050 Uiso 1 1 d D . . H8B H 0.367(3) 0.1244(17) -0.2235(16) 0.050 Uiso 1 1 d D . . H34B H 0.096(2) 0.1960(15) -0.2423(17) 0.050 Uiso 1 1 d D . . H45B H 0.206(3) 0.2590(15) -0.1975(14) 0.050 Uiso 1 1 d D . . H67B H 0.231(3) 0.0823(16) -0.1052(14) 0.050 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02704(13) 0.03803(15) 0.03201(14) 0.00169(13) 0.00272(9) 0.00088(12) S1 0.0396(5) 0.0459(5) 0.0337(5) -0.0040(4) 0.0018(4) 0.0051(4) S2 0.0694(10) 0.1228(15) 0.0785(11) -0.0242(10) -0.0014(8) -0.0239(9) P1 0.0367(5) 0.0333(5) 0.0335(5) 0.0032(4) 0.0053(4) 0.0048(4) P2 0.0328(4) 0.0347(5) 0.0328(5) 0.0044(4) 0.0045(4) -0.0002(4) C1 0.035(2) 0.075(3) 0.057(3) -0.013(2) -0.0051(18) -0.010(2) C2 0.033(2) 0.054(2) 0.076(3) 0.001(2) -0.001(2) -0.0106(17) C3 0.0329(19) 0.071(3) 0.053(2) 0.007(2) 0.0114(18) -0.0082(18) C4 0.0273(18) 0.061(3) 0.070(3) -0.005(2) 0.0068(18) 0.0040(16) C5 0.0314(19) 0.081(3) 0.056(3) 0.010(2) -0.0084(18) 0.0019(19) C11 0.044(2) 0.036(2) 0.052(2) 0.0087(17) 0.0062(18) 0.0021(16) C12 0.054(2) 0.045(2) 0.065(3) 0.001(2) 0.010(2) -0.0088(19) C13 0.064(3) 0.056(3) 0.079(3) -0.002(2) -0.003(3) -0.016(2) C14 0.057(3) 0.071(3) 0.113(4) 0.009(3) 0.011(3) -0.025(2) C15 0.061(3) 0.098(4) 0.088(4) 0.008(3) 0.027(3) -0.024(3) C16 0.051(2) 0.071(3) 0.057(3) 0.009(2) 0.012(2) -0.006(2) C21 0.047(2) 0.0323(18) 0.040(2) 0.0024(15) 0.0072(16) 0.0070(15) C22 0.075(3) 0.051(2) 0.042(2) 0.0149(18) 0.026(2) 0.018(2) C23 0.117(4) 0.060(3) 0.073(3) 0.026(2) 0.058(3) 0.049(3) C24 0.092(3) 0.049(2) 0.077(3) 0.023(2) 0.035(3) 0.034(2) C25 0.104(4) 0.055(3) 0.080(3) 0.033(2) 0.049(3) 0.035(3) C26 0.084(3) 0.052(2) 0.060(3) 0.016(2) 0.039(2) 0.027(2) C31 0.053(2) 0.0359(19) 0.0318(18) 0.0038(14) 0.0105(16) 0.0014(15) C32 0.072(3) 0.071(3) 0.044(2) -0.010(2) 0.002(2) 0.009(2) C33 0.095(4) 0.101(4) 0.048(3) -0.009(3) -0.004(3) 0.002(3) C34 0.126(5) 0.084(4) 0.045(3) -0.026(3) 0.012(3) -0.003(3) C35 0.108(4) 0.055(3) 0.055(3) -0.008(2) 0.026(3) 0.015(3) C36 0.074(3) 0.041(2) 0.044(2) 0.0036(18) 0.0117(19) 0.0139(19) C41 0.047(2) 0.0377(19) 0.0321(19) 0.0033(15) 0.0039(16) 0.0005(16) C42 0.062(3) 0.068(3) 0.057(3) 0.022(2) 0.018(2) 0.012(2) C43 0.105(4) 0.074(3) 0.058(3) 0.024(2) 0.040(3) 0.013(3) C44 0.113(4) 0.071(3) 0.038(3) 0.018(2) 0.005(3) 0.002(3) C45 0.082(3) 0.077(3) 0.048(3) 0.018(2) -0.018(2) -0.010(3) C46 0.058(2) 0.061(3) 0.039(2) 0.0093(19) 0.0002(19) -0.009(2) C51 0.0289(17) 0.0362(18) 0.042(2) 0.0118(15) 0.0054(15) 0.0030(14) C52 0.042(2) 0.0391(19) 0.053(2) 0.0073(17) 0.0077(17) 0.0050(16) C53 0.039(2) 0.056(2) 0.071(3) 0.016(2) 0.000(2) -0.0043(18) C54 0.031(2) 0.085(3) 0.065(3) 0.023(2) 0.010(2) 0.004(2) C55 0.048(2) 0.076(3) 0.047(2) 0.013(2) 0.0155(19) 0.019(2) C56 0.041(2) 0.050(2) 0.042(2) 0.0065(17) 0.0077(16) 0.0093(17) C61 0.0329(18) 0.0397(19) 0.042(2) 0.0035(16) 0.0071(15) -0.0012(14) C62 0.058(2) 0.041(2) 0.045(2) 0.0060(17) 0.0100(19) -0.0005(17) C63 0.064(3) 0.059(3) 0.046(2) -0.009(2) 0.000(2) -0.007(2) C64 0.067(3) 0.053(3) 0.064(3) -0.010(2) 0.000(2) -0.014(2) C65 0.076(3) 0.037(2) 0.074(3) 0.008(2) 0.001(2) -0.009(2) C66 0.052(2) 0.039(2) 0.057(3) 0.0109(18) 0.0007(19) 0.0000(17) B3 0.084(4) 0.095(4) 0.048(3) -0.019(3) -0.008(3) 0.009(3) B4 0.129(6) 0.072(4) 0.037(3) 0.004(3) 0.003(3) 0.012(4) B5 0.071(3) 0.066(3) 0.042(3) 0.003(2) 0.011(2) -0.007(3) B6 0.053(3) 0.051(3) 0.040(2) -0.003(2) 0.005(2) 0.012(2) B7 0.095(4) 0.056(3) 0.049(3) -0.018(2) 0.011(3) -0.005(3) B8 0.054(3) 0.066(3) 0.035(2) -0.004(2) 0.009(2) 0.006(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 C1 2.193(4) . ? Ru1 C2 2.201(3) . ? Ru1 C3 2.215(3) . ? Ru1 C5 2.218(3) . ? Ru1 C4 2.226(3) . ? Ru1 P2 2.3319(9) . ? Ru1 P1 2.3576(9) . ? Ru1 S1 2.4017(9) . ? S1 B5 1.879(5) . ? S1 B6 1.888(4) . ? S2 B3 1.852(7) . ? S2 B7 1.866(6) . ? P1 C31 1.831(3) . ? P1 C11 1.847(4) . ? P1 C21 1.850(3) . ? P2 C51 1.829(3) . ? P2 C61 1.842(3) . ? P2 C41 1.851(3) . ? C1 C5 1.399(6) . ? C1 C2 1.405(5) . ? C1 H1 0.93 . ? C2 C3 1.398(5) . ? C2 H2 0.93 . ? C3 C4 1.416(5) . ? C3 H3 0.93 . ? C4 C5 1.395(5) . ? C4 H4 0.93 . ? C5 H5 0.93 . ? C11 C16 1.383(5) . ? C11 C12 1.394(5) . ? C12 C13 1.392(5) . ? C12 H12 0.93 . ? C13 C14 1.357(6) . ? C13 H13 0.93 . ? C14 C15 1.360(7) . ? C14 H14 0.93 . ? C15 C16 1.395(6) . ? C15 H15 0.93 . ? C16 H16 0.93 . ? C21 C22 1.356(5) . ? C21 C26 1.382(5) . ? C22 C23 1.386(5) . ? C22 H22 0.93 . ? C23 C24 1.354(5) . ? C23 H23 0.93 . ? C24 C25 1.352(5) . ? C24 H24 0.93 . ? C25 C26 1.379(5) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C31 C36 1.379(5) . ? C31 C32 1.390(5) . ? C32 C33 1.397(6) . ? C32 H32 0.93 . ? C33 C34 1.365(7) . ? C33 H33 0.93 . ? C34 C35 1.355(7) . ? C34 H34 0.93 . ? C35 C36 1.386(5) . ? C35 H35 0.93 . ? C36 H36 0.93 . ? C41 C46 1.371(5) . ? C41 C42 1.384(5) . ? C42 C43 1.387(5) . ? C42 H42 0.93 . ? C43 C44 1.370(6) . ? C43 H43 0.93 . ? C44 C45 1.356(6) . ? C44 H44 0.93 . ? C45 C46 1.391(5) . ? C45 H45 0.93 . ? C46 H46 0.93 . ? C51 C56 1.384(5) . ? C51 C52 1.393(5) . ? C52 C53 1.379(5) . ? C52 H52 0.93 . ? C53 C54 1.353(6) . ? C53 H53 0.93 . ? C54 C55 1.378(6) . ? C54 H54 0.93 . ? C55 C56 1.389(5) . ? C55 H55 0.93 . ? C56 H56 0.93 . ? C61 C66 1.383(5) . ? C61 C62 1.389(5) . ? C62 C63 1.389(5) . ? C62 H62 0.93 . ? C63 C64 1.370(5) . ? C63 H63 0.93 . ? C64 C65 1.366(6) . ? C64 H64 0.93 . ? C65 C66 1.392(5) . ? C65 H65 0.93 . ? C66 H66 0.93 . ? B3 B4 1.798(9) . ? B3 B8 1.813(7) . ? B3 B7 1.947(8) . ? B3 H3B 1.06(3) . ? B3 H34B 1.34(3) . ? B4 B8 1.733(7) . ? B4 B5 1.796(8) . ? B4 H4B 1.08(3) . ? B4 H34B 1.31(3) . ? B4 H45B 1.19(3) . ? B5 B8 1.828(7) . ? B5 B6 2.000(7) . ? B5 H5B 1.12(3) . ? B5 H45B 1.33(3) . ? B6 B8 1.791(6) . ? B6 B7 1.814(7) . ? B6 H6B 1.09(3) . ? B6 H67B 1.17(3) . ? B7 B8 1.794(7) . ? B7 H7B 1.05(3) . ? B7 H67B 1.25(3) . ? B8 H8B 1.06(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 C1 Ru1 C2 37.31(14) . . ? C1 Ru1 C3 62.21(15) . . ? C2 Ru1 C3 36.91(14) . . ? C1 Ru1 C5 36.97(14) . . ? C2 Ru1 C5 61.38(15) . . ? C3 Ru1 C5 61.43(15) . . ? C1 Ru1 C4 62.03(15) . . ? C2 Ru1 C4 61.73(14) . . ? C3 Ru1 C4 37.17(14) . . ? C5 Ru1 C4 36.58(14) . . ? C1 Ru1 P2 103.93(12) . . ? C2 Ru1 P2 88.95(11) . . ? C3 Ru1 P2 110.43(11) . . ? C5 Ru1 P2 140.73(12) . . ? C4 Ru1 P2 147.36(10) . . ? C1 Ru1 P1 101.79(12) . . ? C2 Ru1 P1 138.61(12) . . ? C3 Ru1 P1 148.46(11) . . ? C5 Ru1 P1 89.16(11) . . ? C4 Ru1 P1 111.88(11) . . ? P2 Ru1 P1 99.51(3) . . ? C1 Ru1 S1 159.68(11) . . ? C2 Ru1 S1 128.16(12) . . ? C3 Ru1 S1 98.13(11) . . ? C5 Ru1 S1 130.85(12) . . ? C4 Ru1 S1 99.54(11) . . ? P2 Ru1 S1 87.19(3) . . ? P1 Ru1 S1 92.88(3) . . ? B5 S1 B6 64.1(2) . . ? B5 S1 Ru1 116.98(17) . . ? B6 S1 Ru1 114.67(14) . . ? B3 S2 B7 63.2(2) . . ? C31 P1 C11 104.14(17) . . ? C31 P1 C21 101.87(15) . . ? C11 P1 C21 95.32(15) . . ? C31 P1 Ru1 110.12(11) . . ? C11 P1 Ru1 127.52(12) . . ? C21 P1 Ru1 114.39(11) . . ? C51 P2 C61 102.58(15) . . ? C51 P2 C41 101.72(15) . . ? C61 P2 C41 101.89(15) . . ? C51 P2 Ru1 121.20(10) . . ? C61 P2 Ru1 113.57(11) . . ? C41 P2 Ru1 113.46(11) . . ? C5 C1 C2 107.1(4) . . ? C5 C1 Ru1 72.5(2) . . ? C2 C1 Ru1 71.6(2) . . ? C5 C1 H1 126.4 . . ? C2 C1 H1 126.4 . . ? Ru1 C1 H1 121.2 . . ? C3 C2 C1 108.7(4) . . ? C3 C2 Ru1 72.1(2) . . ? C1 C2 Ru1 71.0(2) . . ? C3 C2 H2 125.7 . . ? C1 C2 H2 125.7 . . ? Ru1 C2 H2 122.8 . . ? C2 C3 C4 107.6(3) . . ? C2 C3 Ru1 71.0(2) . . ? C4 C3 Ru1 71.8(2) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? Ru1 C3 H3 122.7 . . ? C5 C4 C3 107.4(4) . . ? C5 C4 Ru1 71.4(2) . . ? C3 C4 Ru1 71.0(2) . . ? C5 C4 H4 126.3 . . ? C3 C4 H4 126.3 . . ? Ru1 C4 H4 122.9 . . ? C4 C5 C1 109.2(4) . . ? C4 C5 Ru1 72.0(2) . . ? C1 C5 Ru1 70.5(2) . . ? C4 C5 H5 125.4 . . ? C1 C5 H5 125.4 . . ? Ru1 C5 H5 123.7 . . ? C16 C11 C12 117.9(4) . . ? C16 C11 P1 124.5(3) . . ? C12 C11 P1 117.3(3) . . ? C13 C12 C11 120.9(4) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 C12 119.9(4) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.4(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 120.6(4) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C11 C16 C15 120.3(4) . . ? C11 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C22 C21 C26 118.1(3) . . ? C22 C21 P1 121.9(3) . . ? C26 C21 P1 120.0(3) . . ? C21 C22 C23 120.6(3) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 121.0(4) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C25 C24 C23 119.0(4) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C24 C25 C26 120.7(4) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C21 120.7(4) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C36 C31 C32 117.6(3) . . ? C36 C31 P1 120.7(3) . . ? C32 C31 P1 121.5(3) . . ? C31 C32 C33 120.6(4) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C34 C33 C32 120.1(5) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C35 C34 C33 120.0(4) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.3(4) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C31 C36 C35 121.3(4) . . ? C31 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C46 C41 C42 117.7(3) . . ? C46 C41 P2 123.1(3) . . ? C42 C41 P2 119.2(3) . . ? C41 C42 C43 121.1(4) . . ? C41 C42 H42 119.5 . . ? C43 C42 H42 119.5 . . ? C44 C43 C42 119.7(4) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C45 C44 C43 120.2(4) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 119.8(4) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C41 C46 C45 121.5(4) . . ? C41 C46 H46 119.3 . . ? C45 C46 H46 119.3 . . ? C56 C51 C52 119.2(3) . . ? C56 C51 P2 122.6(3) . . ? C52 C51 P2 118.1(3) . . ? C53 C52 C51 119.6(4) . . ? C53 C52 H52 120.2 . . ? C51 C52 H52 120.2 . . ? C54 C53 C52 121.0(4) . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? C53 C54 C55 120.4(4) . . ? C53 C54 H54 119.8 . . ? C55 C54 H54 119.8 . . ? C54 C55 C56 119.7(4) . . ? C54 C55 H55 120.2 . . ? C56 C55 H55 120.2 . . ? C51 C56 C55 120.1(4) . . ? C51 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C66 C61 C62 118.2(3) . . ? C66 C61 P2 122.6(3) . . ? C62 C61 P2 119.2(3) . . ? C63 C62 C61 121.2(3) . . ? C63 C62 H62 119.4 . . ? C61 C62 H62 119.4 . . ? C64 C63 C62 119.7(4) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? C65 C64 C63 119.9(4) . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C64 C65 C66 120.7(4) . . ? C64 C65 H65 119.6 . . ? C66 C65 H65 119.6 . . ? C61 C66 C65 120.3(4) . . ? C61 C66 H66 119.9 . . ? C65 C66 H66 119.9 . . ? B4 B3 B8 57.4(3) . . ? B4 B3 S2 128.5(4) . . ? B8 B3 S2 110.0(3) . . ? B4 B3 B7 108.4(4) . . ? B8 B3 B7 56.8(3) . . ? S2 B3 B7 58.8(3) . . ? B4 B3 H3B 109.3(19) . . ? B8 B3 H3B 119.3(18) . . ? S2 B3 H3B 118.0(19) . . ? B7 B3 H3B 125.0(19) . . ? B4 B3 H34B 46.7(12) . . ? B8 B3 H34B 99.4(13) . . ? S2 B3 H34B 98.3(14) . . ? B7 B3 H34B 127.3(15) . . ? H3B B3 H34B 108(2) . . ? B8 B4 B5 62.4(3) . . ? B8 B4 B3 61.7(3) . . ? B5 B4 B3 110.5(4) . . ? B8 B4 H4B 119.5(19) . . ? B5 B4 H4B 122.6(19) . . ? B3 B4 H4B 119.2(18) . . ? B8 B4 H34B 104.5(13) . . ? B5 B4 H34B 118.5(15) . . ? B3 B4 H34B 47.7(12) . . ? H4B B4 H34B 116(2) . . ? B8 B4 H45B 108.4(14) . . ? B5 B4 H45B 47.8(13) . . ? B3 B4 H45B 127.7(17) . . ? H4B B4 H45B 110(2) . . ? H34B B4 H45B 96(2) . . ? B4 B5 B8 57.1(3) . . ? B4 B5 S1 122.9(4) . . ? B8 B5 S1 107.1(3) . . ? B4 B5 B6 105.9(3) . . ? B8 B5 B6 55.6(2) . . ? S1 B5 B6 58.16(18) . . ? B4 B5 H5B 113.4(18) . . ? B8 B5 H5B 116.5(17) . . ? S1 B5 H5B 121.3(17) . . ? B6 B5 H5B 121.3(17) . . ? B4 B5 H45B 41.3(12) . . ? B8 B5 H45B 97.0(12) . . ? S1 B5 H45B 104.2(14) . . ? B6 B5 H45B 130.8(14) . . ? H5B B5 H45B 107(2) . . ? B8 B6 B7 59.7(3) . . ? B8 B6 S1 108.3(3) . . ? B7 B6 S1 119.1(3) . . ? B8 B6 B5 57.4(2) . . ? B7 B6 B5 107.5(3) . . ? S1 B6 B5 57.73(19) . . ? B8 B6 H6B 112.3(17) . . ? B7 B6 H6B 121.2(18) . . ? S1 B6 H6B 118.1(18) . . ? B5 B6 H6B 113.1(18) . . ? B8 B6 H67B 102.7(14) . . ? B7 B6 H67B 43.0(13) . . ? S1 B6 H67B 107.8(16) . . ? B5 B6 H67B 140.2(15) . . ? H6B B6 H67B 106(2) . . ? B8 B7 B6 59.5(3) . . ? B8 B7 S2 110.2(3) . . ? B6 B7 S2 118.9(3) . . ? B8 B7 B3 57.8(3) . . ? B6 B7 B3 106.0(3) . . ? S2 B7 B3 58.1(3) . . ? B8 B7 H7B 108.2(19) . . ? B6 B7 H7B 117.8(19) . . ? S2 B7 H7B 121.9(19) . . ? B3 B7 H7B 115.7(19) . . ? B8 B7 H67B 99.4(13) . . ? B6 B7 H67B 39.9(12) . . ? S2 B7 H67B 107.5(15) . . ? B3 B7 H67B 135.7(15) . . ? H7B B7 H67B 107(2) . . ? B4 B8 B6 118.6(4) . . ? B4 B8 B7 119.0(4) . . ? B6 B8 B7 60.8(3) . . ? B4 B8 B3 60.9(3) . . ? B6 B8 B3 113.0(4) . . ? B7 B8 B3 65.4(3) . . ? B4 B8 B5 60.5(3) . . ? B6 B8 B5 67.1(3) . . ? B7 B8 B5 116.3(3) . . ? B3 B8 B5 108.4(4) . . ? B4 B8 H8B 116.4(18) . . ? B6 B8 H8B 114.9(18) . . ? B7 B8 H8B 115.5(18) . . ? B3 B8 H8B 122.5(18) . . ? B5 B8 H8B 118.1(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ru1 S1 B5 -23.9(4) . . . . ? C2 Ru1 S1 B5 13.9(2) . . . . ? C3 Ru1 S1 B5 -9.9(2) . . . . ? C5 Ru1 S1 B5 -68.9(2) . . . . ? C4 Ru1 S1 B5 -47.5(2) . . . . ? P2 Ru1 S1 B5 100.31(19) . . . . ? P1 Ru1 S1 B5 -160.30(19) . . . . ? C1 Ru1 S1 B6 48.4(4) . . . . ? C2 Ru1 S1 B6 86.1(2) . . . . ? C3 Ru1 S1 B6 62.3(2) . . . . ? C5 Ru1 S1 B6 3.3(2) . . . . ? C4 Ru1 S1 B6 24.7(2) . . . . ? P2 Ru1 S1 B6 172.54(17) . . . . ? P1 Ru1 S1 B6 -88.07(17) . . . . ? C1 Ru1 P1 C31 34.40(17) . . . . ? C2 Ru1 P1 C31 27.2(2) . . . . ? C3 Ru1 P1 C31 89.6(2) . . . . ? C5 Ru1 P1 C31 69.39(17) . . . . ? C4 Ru1 P1 C31 98.78(16) . . . . ? P2 Ru1 P1 C31 -72.11(12) . . . . ? S1 Ru1 P1 C31 -159.75(12) . . . . ? C1 Ru1 P1 C11 161.95(19) . . . . ? C2 Ru1 P1 C11 154.8(2) . . . . ? C3 Ru1 P1 C11 -142.8(3) . . . . ? C5 Ru1 P1 C11 -163.07(19) . . . . ? C4 Ru1 P1 C11 -133.67(19) . . . . ? P2 Ru1 P1 C11 55.43(15) . . . . ? S1 Ru1 P1 C11 -32.20(15) . . . . ? C1 Ru1 P1 C21 -79.59(17) . . . . ? C2 Ru1 P1 C21 -86.8(2) . . . . ? C3 Ru1 P1 C21 -24.4(2) . . . . ? C5 Ru1 P1 C21 -44.61(17) . . . . ? C4 Ru1 P1 C21 -15.22(17) . . . . ? P2 Ru1 P1 C21 173.89(13) . . . . ? S1 Ru1 P1 C21 86.26(13) . . . . ? C1 Ru1 P2 C51 -120.05(18) . . . . ? C2 Ru1 P2 C51 -154.55(17) . . . . ? C3 Ru1 P2 C51 174.80(17) . . . . ? C5 Ru1 P2 C51 -115.7(2) . . . . ? C4 Ru1 P2 C51 -179.5(2) . . . . ? P1 Ru1 P2 C51 -15.28(13) . . . . ? S1 Ru1 P2 C51 77.17(13) . . . . ? C1 Ru1 P2 C61 2.76(17) . . . . ? C2 Ru1 P2 C61 -31.73(16) . . . . ? C3 Ru1 P2 C61 -62.39(17) . . . . ? C5 Ru1 P2 C61 7.1(2) . . . . ? C4 Ru1 P2 C61 -56.7(2) . . . . ? P1 Ru1 P2 C61 107.53(12) . . . . ? S1 Ru1 P2 C61 -160.02(12) . . . . ? C1 Ru1 P2 C41 118.50(17) . . . . ? C2 Ru1 P2 C41 84.01(17) . . . . ? C3 Ru1 P2 C41 53.35(17) . . . . ? C5 Ru1 P2 C41 122.8(2) . . . . ? C4 Ru1 P2 C41 59.1(2) . . . . ? P1 Ru1 P2 C41 -136.73(12) . . . . ? S1 Ru1 P2 C41 -44.28(12) . . . . ? C2 Ru1 C1 C5 -115.4(4) . . . . ? C3 Ru1 C1 C5 -78.5(3) . . . . ? C4 Ru1 C1 C5 -36.3(2) . . . . ? P2 Ru1 C1 C5 175.5(2) . . . . ? P1 Ru1 C1 C5 72.4(2) . . . . ? S1 Ru1 C1 C5 -62.9(5) . . . . ? C3 Ru1 C1 C2 36.9(2) . . . . ? C5 Ru1 C1 C2 115.4(4) . . . . ? C4 Ru1 C1 C2 79.2(3) . . . . ? P2 Ru1 C1 C2 -69.1(2) . . . . ? P1 Ru1 C1 C2 -172.1(2) . . . . ? S1 Ru1 C1 C2 52.5(5) . . . . ? C5 C1 C2 C3 1.6(4) . . . . ? Ru1 C1 C2 C3 -62.7(3) . . . . ? C5 C1 C2 Ru1 64.3(2) . . . . ? C1 Ru1 C2 C3 117.8(3) . . . . ? C5 Ru1 C2 C3 79.6(2) . . . . ? C4 Ru1 C2 C3 37.8(2) . . . . ? P2 Ru1 C2 C3 -127.3(2) . . . . ? P1 Ru1 C2 C3 129.5(2) . . . . ? S1 Ru1 C2 C3 -41.7(3) . . . . ? C3 Ru1 C2 C1 -117.8(3) . . . . ? C5 Ru1 C2 C1 -38.2(2) . . . . ? C4 Ru1 C2 C1 -80.0(3) . . . . ? P2 Ru1 C2 C1 114.9(2) . . . . ? P1 Ru1 C2 C1 11.7(3) . . . . ? S1 Ru1 C2 C1 -159.5(2) . . . . ? C1 C2 C3 C4 -0.9(4) . . . . ? Ru1 C2 C3 C4 -62.9(2) . . . . ? C1 C2 C3 Ru1 62.0(2) . . . . ? C1 Ru1 C3 C2 -37.3(2) . . . . ? C5 Ru1 C3 C2 -79.5(3) . . . . ? C4 Ru1 C3 C2 -116.8(3) . . . . ? P2 Ru1 C3 C2 58.1(2) . . . . ? P1 Ru1 C3 C2 -102.6(3) . . . . ? S1 Ru1 C3 C2 148.1(2) . . . . ? C1 Ru1 C3 C4 79.5(3) . . . . ? C2 Ru1 C3 C4 116.8(3) . . . . ? C5 Ru1 C3 C4 37.3(2) . . . . ? P2 Ru1 C3 C4 174.9(2) . . . . ? P1 Ru1 C3 C4 14.2(4) . . . . ? S1 Ru1 C3 C4 -95.1(2) . . . . ? C2 C3 C4 C5 -0.2(4) . . . . ? Ru1 C3 C4 C5 -62.6(2) . . . . ? C2 C3 C4 Ru1 62.3(2) . . . . ? C1 Ru1 C4 C5 36.6(2) . . . . ? C2 Ru1 C4 C5 79.2(3) . . . . ? C3 Ru1 C4 C5 116.7(3) . . . . ? P2 Ru1 C4 C5 107.8(3) . . . . ? P1 Ru1 C4 C5 -55.4(3) . . . . ? S1 Ru1 C4 C5 -152.4(2) . . . . ? C1 Ru1 C4 C3 -80.0(3) . . . . ? C2 Ru1 C4 C3 -37.5(2) . . . . ? C5 Ru1 C4 C3 -116.7(3) . . . . ? P2 Ru1 C4 C3 -8.9(3) . . . . ? P1 Ru1 C4 C3 -172.1(2) . . . . ? S1 Ru1 C4 C3 90.9(2) . . . . ? C3 C4 C5 C1 1.3(4) . . . . ? Ru1 C4 C5 C1 -61.0(3) . . . . ? C3 C4 C5 Ru1 62.3(2) . . . . ? C2 C1 C5 C4 -1.8(4) . . . . ? Ru1 C1 C5 C4 62.0(3) . . . . ? C2 C1 C5 Ru1 -63.7(2) . . . . ? C1 Ru1 C5 C4 -118.8(4) . . . . ? C2 Ru1 C5 C4 -80.2(3) . . . . ? C3 Ru1 C5 C4 -37.9(2) . . . . ? P2 Ru1 C5 C4 -125.8(2) . . . . ? P1 Ru1 C5 C4 130.2(2) . . . . ? S1 Ru1 C5 C4 37.1(3) . . . . ? C2 Ru1 C5 C1 38.6(2) . . . . ? C3 Ru1 C5 C1 80.8(3) . . . . ? C4 Ru1 C5 C1 118.8(4) . . . . ? P2 Ru1 C5 C1 -7.0(3) . . . . ? P1 Ru1 C5 C1 -111.0(2) . . . . ? S1 Ru1 C5 C1 155.9(2) . . . . ? C31 P1 C11 C16 -7.0(4) . . . . ? C21 P1 C11 C16 96.7(3) . . . . ? Ru1 P1 C11 C16 -136.9(3) . . . . ? C31 P1 C11 C12 -179.9(3) . . . . ? C21 P1 C11 C12 -76.2(3) . . . . ? Ru1 P1 C11 C12 50.3(3) . . . . ? C16 C11 C12 C13 1.3(6) . . . . ? P1 C11 C12 C13 174.6(3) . . . . ? C11 C12 C13 C14 0.3(6) . . . . ? C12 C13 C14 C15 -0.9(7) . . . . ? C13 C14 C15 C16 -0.1(8) . . . . ? C12 C11 C16 C15 -2.2(6) . . . . ? P1 C11 C16 C15 -175.0(3) . . . . ? C14 C15 C16 C11 1.7(7) . . . . ? C31 P1 C21 C22 -138.8(3) . . . . ? C11 P1 C21 C22 115.5(3) . . . . ? Ru1 P1 C21 C22 -20.1(4) . . . . ? C31 P1 C21 C26 44.5(4) . . . . ? C11 P1 C21 C26 -61.2(4) . . . . ? Ru1 P1 C21 C26 163.3(3) . . . . ? C26 C21 C22 C23 -1.8(6) . . . . ? P1 C21 C22 C23 -178.6(4) . . . . ? C21 C22 C23 C24 0.7(8) . . . . ? C22 C23 C24 C25 0.0(8) . . . . ? C23 C24 C25 C26 0.4(8) . . . . ? C24 C25 C26 C21 -1.6(8) . . . . ? C22 C21 C26 C25 2.3(7) . . . . ? P1 C21 C26 C25 179.1(4) . . . . ? C11 P1 C31 C36 -51.6(3) . . . . ? C21 P1 C31 C36 -150.3(3) . . . . ? Ru1 P1 C31 C36 88.0(3) . . . . ? C11 P1 C31 C32 133.9(3) . . . . ? C21 P1 C31 C32 35.2(3) . . . . ? Ru1 P1 C31 C32 -86.6(3) . . . . ? C36 C31 C32 C33 1.3(6) . . . . ? P1 C31 C32 C33 176.0(3) . . . . ? C31 C32 C33 C34 0.5(7) . . . . ? C32 C33 C34 C35 -1.0(8) . . . . ? C33 C34 C35 C36 -0.5(8) . . . . ? C32 C31 C36 C35 -2.8(6) . . . . ? P1 C31 C36 C35 -177.6(3) . . . . ? C34 C35 C36 C31 2.5(7) . . . . ? C51 P2 C41 C46 2.8(3) . . . . ? C61 P2 C41 C46 -102.9(3) . . . . ? Ru1 P2 C41 C46 134.7(3) . . . . ? C51 P2 C41 C42 -178.0(3) . . . . ? C61 P2 C41 C42 76.3(3) . . . . ? Ru1 P2 C41 C42 -46.2(3) . . . . ? C46 C41 C42 C43 0.0(6) . . . . ? P2 C41 C42 C43 -179.2(3) . . . . ? C41 C42 C43 C44 -0.8(7) . . . . ? C42 C43 C44 C45 0.8(7) . . . . ? C43 C44 C45 C46 0.0(7) . . . . ? C42 C41 C46 C45 0.9(6) . . . . ? P2 C41 C46 C45 180.0(3) . . . . ? C44 C45 C46 C41 -0.9(7) . . . . ? C61 P2 C51 C56 -5.5(3) . . . . ? C41 P2 C51 C56 -110.7(3) . . . . ? Ru1 P2 C51 C56 122.4(3) . . . . ? C61 P2 C51 C52 175.6(3) . . . . ? C41 P2 C51 C52 70.5(3) . . . . ? Ru1 P2 C51 C52 -56.5(3) . . . . ? C56 C51 C52 C53 -1.3(5) . . . . ? P2 C51 C52 C53 177.6(3) . . . . ? C51 C52 C53 C54 -0.7(6) . . . . ? C52 C53 C54 C55 1.5(6) . . . . ? C53 C54 C55 C56 -0.3(6) . . . . ? C52 C51 C56 C55 2.5(5) . . . . ? P2 C51 C56 C55 -176.3(3) . . . . ? C54 C55 C56 C51 -1.8(5) . . . . ? C51 P2 C61 C66 -96.5(3) . . . . ? C41 P2 C61 C66 8.5(3) . . . . ? Ru1 P2 C61 C66 130.9(3) . . . . ? C51 P2 C61 C62 83.3(3) . . . . ? C41 P2 C61 C62 -171.6(3) . . . . ? Ru1 P2 C61 C62 -49.2(3) . . . . ? C66 C61 C62 C63 -2.2(5) . . . . ? P2 C61 C62 C63 178.0(3) . . . . ? C61 C62 C63 C64 1.4(6) . . . . ? C62 C63 C64 C65 -0.3(6) . . . . ? C63 C64 C65 C66 -0.1(7) . . . . ? C62 C61 C66 C65 1.7(5) . . . . ? P2 C61 C66 C65 -178.4(3) . . . . ? C64 C65 C66 C61 -0.6(6) . . . . ? B7 S2 B3 B4 -89.3(5) . . . . ? S2A S2 B3 B8 127.0(4) . . . . ? B7 S2 B3 B8 -25.7(3) . . . . ? S2 B3 B4 B8 90.5(5) . . . . ? B7 B3 B4 B8 26.2(4) . . . . ? B8 B3 B4 B5 -40.3(4) . . . . ? S2 B3 B4 B5 50.2(7) . . . . ? B7 B3 B4 B5 -14.1(6) . . . . ? B3 B4 B5 B8 40.0(4) . . . . ? B8 B4 B5 S1 -90.0(4) . . . . ? B3 B4 B5 S1 -50.0(6) . . . . ? B8 B4 B5 B6 -28.0(3) . . . . ? B3 B4 B5 B6 12.0(5) . . . . ? B6 S1 B5 B4 88.9(4) . . . . ? Ru1 S1 B5 B4 -165.2(3) . . . . ? B6 S1 B5 B8 27.4(3) . . . . ? Ru1 S1 B5 B8 133.3(2) . . . . ? Ru1 S1 B5 B6 105.87(19) . . . . ? B5 S1 B6 B8 -28.2(3) . . . . ? Ru1 S1 B6 B8 -137.6(2) . . . . ? B5 S1 B6 B7 -93.1(4) . . . . ? Ru1 S1 B6 B7 157.5(3) . . . . ? Ru1 S1 B6 B5 -109.4(2) . . . . ? B4 B5 B6 B8 28.5(4) . . . . ? S1 B5 B6 B8 147.8(3) . . . . ? B4 B5 B6 B7 -5.4(5) . . . . ? B8 B5 B6 B7 -33.9(3) . . . . ? S1 B5 B6 B7 113.9(3) . . . . ? B4 B5 B6 S1 -119.3(4) . . . . ? B8 B5 B6 S1 -147.8(3) . . . . ? S1 B6 B7 B8 95.2(3) . . . . ? B5 B6 B7 B8 33.0(3) . . . . ? B8 B6 B7 S2 -97.6(4) . . . . ? S1 B6 B7 S2 -2.4(5) . . . . ? B5 B6 B7 S2 -64.7(4) . . . . ? B8 B6 B7 B3 -35.7(3) . . . . ? S1 B6 B7 B3 59.6(4) . . . . ? B5 B6 B7 B3 -2.7(4) . . . . ? B3 S2 B7 B8 26.0(3) . . . . ? B3 S2 B7 B6 91.6(4) . . . . ? B4 B3 B7 B8 -26.4(4) . . . . ? S2 B3 B7 B8 -150.9(3) . . . . ? B4 B3 B7 B6 10.1(5) . . . . ? B8 B3 B7 B6 36.4(3) . . . . ? S2 B3 B7 B6 -114.4(3) . . . . ? B4 B3 B7 S2 124.5(4) . . . . ? B8 B3 B7 S2 150.9(3) . . . . ? B5 B4 B8 B6 35.0(4) . . . . ? B3 B4 B8 B6 -101.9(4) . . . . ? B5 B4 B8 B7 105.5(4) . . . . ? B3 B4 B8 B7 -31.3(4) . . . . ? B5 B4 B8 B3 136.9(4) . . . . ? B3 B4 B8 B5 -136.9(4) . . . . ? B7 B6 B8 B4 109.1(5) . . . . ? S1 B6 B8 B4 -4.4(5) . . . . ? B5 B6 B8 B4 -32.8(4) . . . . ? S1 B6 B8 B7 -113.6(3) . . . . ? B5 B6 B8 B7 -141.9(4) . . . . ? B7 B6 B8 B3 40.8(4) . . . . ? S1 B6 B8 B3 -72.7(4) . . . . ? B5 B6 B8 B3 -101.1(4) . . . . ? B7 B6 B8 B5 141.9(4) . . . . ? S1 B6 B8 B5 28.4(3) . . . . ? B6 B7 B8 B4 -108.5(4) . . . . ? S2 B7 B8 B4 3.9(5) . . . . ? B3 B7 B8 B4 30.0(4) . . . . ? S2 B7 B8 B6 112.4(3) . . . . ? B3 B7 B8 B6 138.5(4) . . . . ? B6 B7 B8 B3 -138.5(4) . . . . ? S2 B7 B8 B3 -26.1(3) . . . . ? B6 B7 B8 B5 -39.3(4) . . . . ? S2 B7 B8 B5 73.1(4) . . . . ? B3 B7 B8 B5 99.2(4) . . . . ? S2 B3 B8 B4 -123.7(4) . . . . ? B7 B3 B8 B4 -150.0(4) . . . . ? B4 B3 B8 B6 111.0(4) . . . . ? S2 B3 B8 B6 -12.6(5) . . . . ? B7 B3 B8 B6 -38.9(3) . . . . ? B4 B3 B8 B7 150.0(4) . . . . ? S2 B3 B8 B7 26.3(3) . . . . ? B4 B3 B8 B5 38.8(4) . . . . ? S2 B3 B8 B5 -84.9(4) . . . . ? B7 B3 B8 B5 -111.2(3) . . . . ? S1 B5 B8 B4 118.6(4) . . . . ? B6 B5 B8 B4 146.9(4) . . . . ? B4 B5 B8 B6 -146.9(4) . . . . ? S1 B5 B8 B6 -28.3(3) . . . . ? B4 B5 B8 B7 -110.0(5) . . . . ? S1 B5 B8 B7 8.6(5) . . . . ? B6 B5 B8 B7 36.9(3) . . . . ? B4 B5 B8 B3 -39.0(4) . . . . ? S1 B5 B8 B3 79.6(4) . . . . ? B6 B5 B8 B3 107.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.590 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.079 #========================================================================= # END of CIF for Compound 2 #========================================================================= data_compd-4 _database_code_depnum_ccdc_archive 'CCDC 264504' #================================================================ # 5. Chemical Data _chemical_name_systematic ; ? #Insert the chemical name here. ; _chemical_name_common ? _chemical_formula_moiety 'C23 H33 B6 P Ru S2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C23 H33 B6 P Ru S2' _chemical_formula_weight 570.51 _chemical_compound_source 'synthesized by the authors, see text' 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' B B 0.0013 0.0007 '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' 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' #===================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.0430(10) _cell_length_b 10.1578(7) _cell_length_c 24.528(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.168(7) _cell_angle_gamma 90.00 _cell_volume 2744.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 294(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.61 _cell_measurement_theta_max 17.44 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description 'plate cut from a larger piece' _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.24 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method ? _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type empirical # psi-scans at 4\% steps (North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details '(North, Philips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.7207 _exptl_absorpt_correction_T_max 0.8281 #===================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? #Insert any special details here. ; _diffrn_ambient_temperature 294(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 1.8 _diffrn_reflns_number 6764 _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.39 _reflns_number_total 6264 _reflns_number_gt 4115 _reflns_threshold_expression >2\s(I) _computing_data_collection 'DIFRAC (Gabe & White, 1993)' _computing_cell_refinement 'DIFRAC (Gabe & White, 1993)' _computing_data_reduction 'DATRD2 in NRCVAX94 (Gabe, Le Page, Charland, Lee & White, 1989)' _computing_structure_solution 'Patterson heavy-atom method and NRCVAX94' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'NRCVAX94, SHELXL97' #==================================================================== _refine_special_details ; Molecule (I) crystallised in the monoclinic system; space group P2~1~/c from the systematic absences. Boron cage H atoms were located from a difference synthesis and their coordinates adjusted to give a normalised B-H distance of 1.10\%A; these H atom contributions were then included but not refined in the final calculations. C-H hydrogen atoms were treated as riding atoms (C-H 0.93 to 0.98\%A). ; # 8. Refinement Data _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0669P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0022(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6264 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _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 Ru5 Ru 0.20271(3) 0.09869(3) 0.228674(13) 0.03412(12) Uani 1 1 d . . . P1 P 0.18200(10) 0.26748(13) -0.00002(5) 0.0436(3) Uani 1 1 d . . . S4 S 0.17210(10) 0.31143(11) 0.19100(5) 0.0412(3) Uani 1 1 d . . . S6 S 0.27982(11) -0.01661(13) 0.15422(5) 0.0517(3) Uani 1 1 d . . . B1 B 0.0531(4) 0.1785(5) 0.1685(2) 0.0398(11) Uani 1 1 d . . . H1 H -0.0361 0.1856 0.1855 0.048 Uiso 1 1 calc R . . B2 B 0.1084(5) 0.0139(5) 0.1500(2) 0.0417(11) Uani 1 1 d . . . H2 H 0.0508 -0.0722 0.1566 0.050 Uiso 1 1 calc R . . B3 B 0.0739(4) 0.1365(5) 0.0992(2) 0.0410(11) Uani 1 1 d . . . H3 H -0.0086 0.1204 0.0722 0.049 Uiso 1 1 calc R . . B7 B 0.1977(5) 0.0394(6) 0.0880(2) 0.0493(13) Uani 1 1 d . . . B8 B 0.2026(4) 0.2119(5) 0.0741(2) 0.0408(11) Uani 1 1 d . . . B9 B 0.1110(4) 0.2979(5) 0.1174(2) 0.0421(11) Uani 1 1 d . . . H7 H 0.1966 -0.0410 0.0580 0.060 Uiso 1 1 d . . . H8 H 0.2966 0.2291 0.0907 0.060 Uiso 1 1 d . . . H9 H 0.0505 0.3812 0.1064 0.060 Uiso 1 1 d . . . C1 C 0.3361(4) 0.0181(6) 0.2928(2) 0.0547(13) Uani 1 1 d . . . C2 C 0.2394(5) -0.0718(5) 0.28200(19) 0.0498(12) Uani 1 1 d . . . H2A H 0.2568 -0.1585 0.2732 0.060 Uiso 1 1 calc R . . C3 C 0.1174(4) -0.0332(4) 0.28423(18) 0.0422(10) Uani 1 1 d . . . H3A H 0.0555 -0.0935 0.2758 0.051 Uiso 1 1 calc R . . C4 C 0.0884(4) 0.0968(5) 0.29914(17) 0.0448(10) Uani 1 1 d . . . C5 C 0.1846(5) 0.1864(5) 0.30916(18) 0.0505(12) Uani 1 1 d . . . H5 H 0.1675 0.2732 0.3178 0.061 Uiso 1 1 calc R . . C6 C 0.3066(5) 0.1471(6) 0.30637(19) 0.0561(13) Uani 1 1 d . . . H6 H 0.3684 0.2082 0.3137 0.067 Uiso 1 1 calc R . . C7 C 0.4669(5) -0.0308(7) 0.2891(3) 0.0782(19) Uani 1 1 d . . . H7A H 0.4654 -0.0939 0.2588 0.094 Uiso 1 1 calc R . . C8 C 0.5561(6) 0.0762(9) 0.2767(4) 0.126(3) Uani 1 1 d . . . H8A H 0.5224 0.1292 0.2469 0.188 Uiso 1 1 calc R . . H8B H 0.6305 0.0369 0.2668 0.188 Uiso 1 1 calc R . . H8C H 0.5721 0.1305 0.3084 0.188 Uiso 1 1 calc R . . C9 C 0.5031(7) -0.1076(10) 0.3416(3) 0.136(4) Uani 1 1 d . . . H9A H 0.4432 -0.1739 0.3470 0.203 Uiso 1 1 calc R . . H9B H 0.5082 -0.0483 0.3721 0.203 Uiso 1 1 calc R . . H9C H 0.5806 -0.1487 0.3385 0.203 Uiso 1 1 calc R . . C10 C -0.0425(5) 0.1381(5) 0.3027(2) 0.0568(13) Uani 1 1 d . . . H10A H -0.0679 0.1167 0.3383 0.085 Uiso 1 1 calc R . . H10B H -0.0929 0.0925 0.2754 0.085 Uiso 1 1 calc R . . H10C H -0.0497 0.2313 0.2968 0.085 Uiso 1 1 calc R . . C11 C 0.2307(4) 0.4375(5) -0.00730(19) 0.0472(11) Uani 1 1 d . . . C12 C 0.2703(5) 0.5107(6) 0.0383(2) 0.0688(16) Uani 1 1 d . . . H12 H 0.2777 0.4704 0.0724 0.083 Uiso 1 1 calc R . . C13 C 0.2990(6) 0.6439(6) 0.0339(3) 0.086(2) Uani 1 1 d . . . H13 H 0.3237 0.6924 0.0649 0.103 Uiso 1 1 calc R . . C14 C 0.2905(5) 0.7022(6) -0.0163(3) 0.0746(17) Uani 1 1 d . . . H14 H 0.3145 0.7893 -0.0201 0.090 Uiso 1 1 calc R . . C15 C 0.2465(6) 0.6321(6) -0.0613(3) 0.0763(18) Uani 1 1 d . . . H15 H 0.2357 0.6737 -0.0951 0.092 Uiso 1 1 calc R . . C16 C 0.2182(6) 0.5005(6) -0.0570(2) 0.0683(15) Uani 1 1 d . . . H16 H 0.1902 0.4539 -0.0880 0.082 Uiso 1 1 calc R . . C21 C 0.2692(4) 0.1698(5) -0.04481(18) 0.0467(11) Uani 1 1 d . . . C22 C 0.3945(5) 0.1777(7) -0.0399(3) 0.092(2) Uani 1 1 d . . . H22 H 0.4330 0.2381 -0.0160 0.111 Uiso 1 1 calc R . . C23 C 0.4619(6) 0.0956(8) -0.0705(4) 0.115(3) Uani 1 1 d . . . H23 H 0.5462 0.1010 -0.0666 0.138 Uiso 1 1 calc R . . C24 C 0.4091(6) 0.0071(6) -0.1063(3) 0.0797(18) Uani 1 1 d . . . H24 H 0.4562 -0.0478 -0.1265 0.096 Uiso 1 1 calc R . . C25 C 0.2859(6) 0.0003(5) -0.1120(2) 0.0712(16) Uani 1 1 d . . . H25 H 0.2483 -0.0585 -0.1369 0.085 Uiso 1 1 calc R . . C26 C 0.2158(5) 0.0806(5) -0.0811(2) 0.0583(13) Uani 1 1 d . . . H26 H 0.1316 0.0739 -0.0849 0.070 Uiso 1 1 calc R . . C31 C 0.0268(4) 0.2653(6) -0.0295(2) 0.0626(15) Uani 1 1 d . . . H31A H -0.0222 0.3214 -0.0085 0.094 Uiso 1 1 calc R . . H31B H -0.0041 0.1770 -0.0290 0.094 Uiso 1 1 calc R . . H31C H 0.0244 0.2964 -0.0665 0.094 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 Ru5 0.03448(18) 0.03433(18) 0.03322(18) -0.00005(16) 0.00016(12) -0.00167(16) P1 0.0358(6) 0.0584(8) 0.0361(6) 0.0045(6) -0.0004(5) -0.0088(5) S4 0.0481(6) 0.0339(5) 0.0413(6) -0.0031(5) 0.0012(5) 0.0001(5) S6 0.0604(7) 0.0508(7) 0.0443(7) -0.0007(6) 0.0058(5) 0.0196(6) B1 0.033(2) 0.047(3) 0.040(3) 0.002(2) 0.005(2) 0.001(2) B2 0.048(3) 0.036(3) 0.041(3) -0.002(2) -0.001(2) -0.004(2) B3 0.039(3) 0.046(3) 0.036(3) 0.001(2) -0.004(2) -0.010(2) B7 0.061(3) 0.044(3) 0.043(3) -0.007(2) 0.004(3) 0.001(3) B8 0.038(2) 0.047(3) 0.037(3) 0.003(2) 0.002(2) -0.008(2) B9 0.040(3) 0.039(3) 0.046(3) 0.007(2) -0.003(2) -0.001(2) C1 0.049(3) 0.071(4) 0.042(3) 0.013(3) -0.009(2) 0.002(3) C2 0.059(3) 0.047(3) 0.042(3) 0.009(2) -0.002(2) 0.006(2) C3 0.045(2) 0.037(2) 0.044(3) 0.007(2) 0.0055(19) -0.001(2) C4 0.055(3) 0.043(2) 0.037(2) 0.004(2) 0.0077(19) 0.000(2) C5 0.075(3) 0.044(3) 0.033(2) -0.006(2) 0.007(2) -0.005(2) C6 0.061(3) 0.066(3) 0.039(3) 0.001(2) -0.011(2) -0.015(3) C7 0.047(3) 0.116(5) 0.070(4) 0.025(4) -0.006(3) 0.012(3) C8 0.055(4) 0.160(9) 0.163(8) 0.039(7) 0.018(5) -0.002(5) C9 0.079(5) 0.217(11) 0.110(6) 0.082(7) 0.000(4) 0.058(6) C10 0.069(3) 0.049(3) 0.055(3) 0.002(2) 0.027(3) 0.006(2) C11 0.041(2) 0.056(3) 0.045(3) 0.009(2) 0.003(2) -0.005(2) C12 0.079(4) 0.068(4) 0.057(3) 0.016(3) -0.011(3) -0.028(3) C13 0.109(5) 0.073(4) 0.072(4) 0.014(3) -0.021(4) -0.042(4) C14 0.075(4) 0.071(4) 0.077(4) 0.020(3) 0.001(3) -0.022(3) C15 0.107(5) 0.065(4) 0.058(4) 0.015(3) 0.011(3) 0.004(3) C16 0.103(4) 0.061(3) 0.041(3) 0.003(3) 0.009(3) -0.002(3) C21 0.045(2) 0.058(3) 0.036(2) 0.000(2) 0.0018(19) -0.014(2) C22 0.048(3) 0.119(6) 0.111(5) -0.065(5) 0.018(3) -0.022(4) C23 0.063(4) 0.134(7) 0.153(7) -0.084(6) 0.036(4) -0.028(4) C24 0.082(4) 0.072(4) 0.089(5) -0.023(4) 0.031(4) -0.010(3) C25 0.099(5) 0.047(3) 0.066(4) -0.014(3) -0.003(3) -0.008(3) C26 0.059(3) 0.057(3) 0.057(3) 0.005(3) -0.007(2) -0.015(3) C31 0.042(3) 0.101(4) 0.044(3) 0.012(3) -0.006(2) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. Details ex SHELXL.lst file Mean plane calculations show that atom Ru5 is 1.691(2)\%A from the best plane through atoms C1-C6 of the p-cymene aromatic ring. ; 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 Ru5 C3 2.174(4) . ? Ru5 C5 2.188(4) . ? Ru5 C2 2.190(4) . ? Ru5 C6 2.207(5) . ? Ru5 C4 2.213(4) . ? Ru5 C1 2.232(4) . ? Ru5 B1 2.283(5) . ? Ru5 B2 2.294(5) . ? Ru5 S4 2.3649(11) . ? Ru5 S6 2.3786(12) . ? P1 C21 1.809(5) . ? P1 C31 1.811(5) . ? P1 C11 1.822(5) . ? P1 B8 1.903(5) . ? S4 B9 1.885(5) . ? S4 B1 1.936(5) . ? S6 B7 1.889(6) . ? S6 B2 1.914(5) . ? B1 B3 1.782(7) . ? B1 B2 1.848(7) . ? B1 B9 1.888(7) . ? B1 H1 1.10 . ? B2 B3 1.782(7) . ? B2 B7 1.889(8) . ? B2 H2 1.10 . ? B3 B7 1.724(8) . ? B3 B9 1.740(7) . ? B3 B8 1.764(7) . ? B3 H3 1.10 . ? B7 B8 1.787(8) . ? B7 H7 1.10 . ? B8 B9 1.752(7) . ? B8 H8 1.10 . ? B9 H9 1.10 . ? C1 C6 1.397(8) . ? C1 C2 1.416(7) . ? C1 C7 1.536(7) . ? C2 C3 1.408(6) . ? C2 H2A 0.93 . ? C3 C4 1.413(6) . ? C3 H3A 0.93 . ? C4 C5 1.407(6) . ? C4 C10 1.514(6) . ? C5 C6 1.411(7) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C8 1.513(9) . ? C7 C9 1.534(8) . ? C7 H7A 0.98 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? C11 C16 1.374(7) . ? C11 C12 1.386(7) . ? C12 C13 1.395(8) . ? C12 H12 0.93 . ? C13 C14 1.364(8) . ? C13 H13 0.93 . ? C14 C15 1.372(8) . ? C14 H14 0.93 . ? C15 C16 1.378(8) . ? C15 H15 0.93 . ? C16 H16 0.93 . ? C21 C26 1.372(7) . ? C21 C22 1.382(7) . ? C22 C23 1.377(9) . ? C22 H22 0.93 . ? C23 C24 1.358(9) . ? C23 H23 0.93 . ? C24 C25 1.359(8) . ? C24 H24 0.93 . ? C25 C26 1.388(8) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C31 H31A 0.96 . ? C31 H31B 0.96 . ? C31 H31C 0.96 . ? 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 C3 Ru5 C5 67.23(17) . . ? C3 Ru5 C2 37.63(17) . . ? C5 Ru5 C2 78.94(18) . . ? C3 Ru5 C6 79.50(18) . . ? C5 Ru5 C6 37.44(19) . . ? C2 Ru5 C6 66.35(19) . . ? C3 Ru5 C4 37.56(16) . . ? C5 Ru5 C4 37.28(17) . . ? C2 Ru5 C4 67.54(18) . . ? C6 Ru5 C4 67.52(19) . . ? C3 Ru5 C1 68.02(18) . . ? C5 Ru5 C1 67.2(2) . . ? C2 Ru5 C1 37.34(18) . . ? C6 Ru5 C1 36.7(2) . . ? C4 Ru5 C1 80.26(18) . . ? C3 Ru5 B1 107.34(17) . . ? C5 Ru5 B1 109.25(19) . . ? C2 Ru5 B1 139.52(18) . . ? C6 Ru5 B1 141.8(2) . . ? C4 Ru5 B1 94.66(17) . . ? C1 Ru5 B1 174.83(18) . . ? C3 Ru5 B2 96.05(18) . . ? C5 Ru5 B2 147.84(19) . . ? C2 Ru5 B2 104.99(18) . . ? C6 Ru5 B2 170.43(19) . . ? C4 Ru5 B2 113.84(18) . . ? C1 Ru5 B2 133.8(2) . . ? B1 Ru5 B2 47.63(18) . . ? C3 Ru5 S4 138.75(12) . . ? C5 Ru5 S4 87.75(13) . . ? C2 Ru5 S4 166.14(13) . . ? C6 Ru5 S4 100.62(15) . . ? C4 Ru5 S4 103.86(12) . . ? C1 Ru5 S4 132.77(15) . . ? B1 Ru5 S4 49.20(13) . . ? B2 Ru5 S4 88.33(13) . . ? C3 Ru5 S6 111.94(13) . . ? C5 Ru5 S6 162.62(14) . . ? C2 Ru5 S6 90.47(13) . . ? C6 Ru5 S6 125.45(15) . . ? C4 Ru5 S6 148.39(13) . . ? C1 Ru5 S6 96.08(15) . . ? B1 Ru5 S6 87.77(13) . . ? B2 Ru5 S6 48.32(13) . . ? S4 Ru5 S6 101.47(4) . . ? C21 P1 C31 106.3(2) . . ? C21 P1 C11 106.6(2) . . ? C31 P1 C11 104.5(2) . . ? C21 P1 B8 112.7(2) . . ? C31 P1 B8 114.9(2) . . ? C11 P1 B8 111.1(2) . . ? B9 S4 B1 59.2(2) . . ? B9 S4 Ru5 109.79(16) . . ? B1 S4 Ru5 63.19(15) . . ? B7 S6 B2 59.6(2) . . ? B7 S6 Ru5 109.61(18) . . ? B2 S6 Ru5 63.52(15) . . ? B3 B1 B2 58.8(3) . . ? B3 B1 B9 56.5(3) . . ? B2 B1 B9 106.5(3) . . ? B3 B1 S4 107.9(3) . . ? B2 B1 S4 118.1(3) . . ? B9 B1 S4 59.1(2) . . ? B3 B1 Ru5 113.2(3) . . ? B2 B1 Ru5 66.5(2) . . ? B9 B1 Ru5 113.1(3) . . ? S4 B1 Ru5 67.61(15) . . ? B3 B1 H1 123.9 . . ? B2 B1 H1 118.2 . . ? B9 B1 H1 124.4 . . ? S4 B1 H1 117.1 . . ? Ru5 B1 H1 113.9 . . ? B3 B2 B1 58.8(3) . . ? B3 B2 B7 55.9(3) . . ? B1 B2 B7 106.0(3) . . ? B3 B2 S6 108.2(3) . . ? B1 B2 S6 118.4(3) . . ? B7 B2 S6 59.6(2) . . ? B3 B2 Ru5 112.7(3) . . ? B1 B2 Ru5 65.9(2) . . ? B7 B2 Ru5 113.2(3) . . ? S6 B2 Ru5 68.16(16) . . ? B3 B2 H2 124.2 . . ? B1 B2 H2 118.6 . . ? B7 B2 H2 124.6 . . ? S6 B2 H2 116.3 . . ? Ru5 B2 H2 114.0 . . ? B7 B3 B9 113.9(4) . . ? B7 B3 B8 61.6(3) . . ? B9 B3 B8 60.0(3) . . ? B7 B3 B2 65.2(3) . . ? B9 B3 B2 116.4(3) . . ? B8 B3 B2 114.2(4) . . ? B7 B3 B1 116.6(4) . . ? B9 B3 B1 64.8(3) . . ? B8 B3 B1 113.1(3) . . ? B2 B3 B1 62.5(3) . . ? B7 B3 H3 116.7 . . ? B9 B3 H3 117.6 . . ? B8 B3 H3 120.4 . . ? B2 B3 H3 116.3 . . ? B1 B3 H3 116.9 . . ? B3 B7 B8 60.3(3) . . ? B3 B7 B2 58.9(3) . . ? B8 B7 B2 108.2(4) . . ? B3 B7 S6 111.8(3) . . ? B8 B7 S6 116.1(3) . . ? B2 B7 S6 60.9(2) . . ? B3 B7 H7 124.2 . . ? B8 B7 H7 126.9 . . ? B2 B7 H7 117.2 . . ? S6 B7 H7 109.5 . . ? B9 B8 B3 59.3(3) . . ? B9 B8 B7 110.3(4) . . ? B3 B8 B7 58.1(3) . . ? B9 B8 P1 113.4(3) . . ? B3 B8 P1 114.8(3) . . ? B7 B8 P1 118.0(3) . . ? B9 B8 H8 105.6 . . ? B3 B8 H8 134.6 . . ? B7 B8 H8 97.3 . . ? P1 B8 H8 110.5 . . ? B3 B9 B8 60.7(3) . . ? B3 B9 S4 112.0(3) . . ? B8 B9 S4 115.7(3) . . ? B3 B9 B1 58.7(3) . . ? B8 B9 B1 108.7(3) . . ? S4 B9 B1 61.7(2) . . ? B3 B9 H9 122.3 . . ? B8 B9 H9 127.0 . . ? S4 B9 H9 110.4 . . ? B1 B9 H9 115.4 . . ? C6 C1 C2 117.6(5) . . ? C6 C1 C7 123.7(5) . . ? C2 C1 C7 118.7(5) . . ? C6 C1 Ru5 70.7(3) . . ? C2 C1 Ru5 69.7(3) . . ? C7 C1 Ru5 130.7(4) . . ? C3 C2 C1 121.6(5) . . ? C3 C2 Ru5 70.5(2) . . ? C1 C2 Ru5 72.9(3) . . ? C3 C2 H2A 119.2 . . ? C1 C2 H2A 119.2 . . ? Ru5 C2 H2A 130.0 . . ? C2 C3 C4 120.4(4) . . ? C2 C3 Ru5 71.8(3) . . ? C4 C3 Ru5 72.7(2) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? Ru5 C3 H3A 127.8 . . ? C5 C4 C3 117.8(4) . . ? C5 C4 C10 121.5(4) . . ? C3 C4 C10 120.6(4) . . ? C5 C4 Ru5 70.4(3) . . ? C3 C4 Ru5 69.7(2) . . ? C10 C4 Ru5 130.1(3) . . ? C4 C5 C6 121.3(5) . . ? C4 C5 Ru5 72.3(3) . . ? C6 C5 Ru5 72.0(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? Ru5 C5 H5 128.7 . . ? C1 C6 C5 121.1(5) . . ? C1 C6 Ru5 72.6(3) . . ? C5 C6 Ru5 70.5(3) . . ? C1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? Ru5 C6 H6 130.0 . . ? C8 C7 C9 113.6(6) . . ? C8 C7 C1 114.1(6) . . ? C9 C7 C1 107.6(5) . . ? C8 C7 H7A 107.0 . . ? C9 C7 H7A 107.0 . . ? C1 C7 H7A 107.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 118.1(5) . . ? C16 C11 P1 121.1(4) . . ? C12 C11 P1 120.5(4) . . ? C11 C12 C13 121.2(5) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C14 C13 C12 119.3(6) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 119.8(6) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 120.7(6) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C11 C16 C15 120.7(6) . . ? C11 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C26 C21 C22 118.4(5) . . ? C26 C21 P1 122.2(4) . . ? C22 C21 P1 119.3(4) . . ? C23 C22 C21 119.7(6) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 121.9(6) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 C24 C25 118.7(6) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C24 C25 C26 120.5(5) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C21 C26 C25 120.8(5) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? P1 C31 H31A 109.5 . . ? P1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Ru5 S4 B9 -104.9(3) . . . . ? C5 Ru5 S4 B9 -155.7(2) . . . . ? C2 Ru5 S4 B9 -171.8(6) . . . . ? C6 Ru5 S4 B9 169.0(2) . . . . ? C4 Ru5 S4 B9 -121.8(2) . . . . ? C1 Ru5 S4 B9 148.7(3) . . . . ? B1 Ru5 S4 B9 -37.7(2) . . . . ? B2 Ru5 S4 B9 -7.6(2) . . . . ? S6 Ru5 S4 B9 39.16(18) . . . . ? C3 Ru5 S4 B1 -67.2(3) . . . . ? C5 Ru5 S4 B1 -118.0(2) . . . . ? C2 Ru5 S4 B1 -134.1(6) . . . . ? C6 Ru5 S4 B1 -153.4(2) . . . . ? C4 Ru5 S4 B1 -84.1(2) . . . . ? C1 Ru5 S4 B1 -173.6(2) . . . . ? B2 Ru5 S4 B1 30.1(2) . . . . ? S6 Ru5 S4 B1 76.84(17) . . . . ? C3 Ru5 S6 B7 117.0(2) . . . . ? C5 Ru5 S6 B7 -159.3(5) . . . . ? C2 Ru5 S6 B7 148.7(2) . . . . ? C6 Ru5 S6 B7 -150.4(3) . . . . ? C4 Ru5 S6 B7 104.4(3) . . . . ? C1 Ru5 S6 B7 -174.3(2) . . . . ? B1 Ru5 S6 B7 9.2(2) . . . . ? B2 Ru5 S6 B7 38.9(3) . . . . ? S4 Ru5 S6 B7 -38.4(2) . . . . ? C3 Ru5 S6 B2 78.1(2) . . . . ? C5 Ru5 S6 B2 161.8(5) . . . . ? C2 Ru5 S6 B2 109.8(2) . . . . ? C6 Ru5 S6 B2 170.7(2) . . . . ? C4 Ru5 S6 B2 65.5(3) . . . . ? C1 Ru5 S6 B2 146.8(2) . . . . ? B1 Ru5 S6 B2 -29.7(2) . . . . ? S4 Ru5 S6 B2 -77.26(18) . . . . ? B9 S4 B1 B3 29.6(3) . . . . ? Ru5 S4 B1 B3 -108.3(3) . . . . ? B9 S4 B1 B2 93.2(4) . . . . ? Ru5 S4 B1 B2 -44.8(3) . . . . ? Ru5 S4 B1 B9 -138.0(2) . . . . ? B9 S4 B1 Ru5 138.0(2) . . . . ? C3 Ru5 B1 B3 -118.9(3) . . . . ? C5 Ru5 B1 B3 169.8(3) . . . . ? C2 Ru5 B1 B3 -94.7(4) . . . . ? C6 Ru5 B1 B3 146.0(3) . . . . ? C4 Ru5 B1 B3 -155.0(3) . . . . ? B2 Ru5 B1 B3 -36.7(3) . . . . ? S4 Ru5 B1 B3 100.6(3) . . . . ? S6 Ru5 B1 B3 -6.6(3) . . . . ? C3 Ru5 B1 B2 -82.2(2) . . . . ? C5 Ru5 B1 B2 -153.5(2) . . . . ? C2 Ru5 B1 B2 -58.0(4) . . . . ? C6 Ru5 B1 B2 -177.2(3) . . . . ? C4 Ru5 B1 B2 -118.3(2) . . . . ? S4 Ru5 B1 B2 137.3(3) . . . . ? S6 Ru5 B1 B2 30.1(2) . . . . ? C3 Ru5 B1 B9 179.1(3) . . . . ? C5 Ru5 B1 B9 107.8(3) . . . . ? C2 Ru5 B1 B9 -156.7(3) . . . . ? C6 Ru5 B1 B9 84.1(4) . . . . ? C4 Ru5 B1 B9 143.0(3) . . . . ? B2 Ru5 B1 B9 -98.7(4) . . . . ? S4 Ru5 B1 B9 38.6(2) . . . . ? S6 Ru5 B1 B9 -68.6(3) . . . . ? C3 Ru5 B1 S4 140.44(15) . . . . ? C5 Ru5 B1 S4 69.12(19) . . . . ? C2 Ru5 B1 S4 164.6(2) . . . . ? C6 Ru5 B1 S4 45.4(3) . . . . ? C4 Ru5 B1 S4 104.32(17) . . . . ? B2 Ru5 B1 S4 -137.3(3) . . . . ? S6 Ru5 B1 S4 -107.26(12) . . . . ? B9 B1 B2 B3 -31.5(3) . . . . ? S4 B1 B2 B3 -94.7(4) . . . . ? Ru5 B1 B2 B3 -140.0(3) . . . . ? B3 B1 B2 B7 31.3(3) . . . . ? B9 B1 B2 B7 -0.2(4) . . . . ? S4 B1 B2 B7 -63.5(4) . . . . ? Ru5 B1 B2 B7 -108.7(3) . . . . ? B3 B1 B2 S6 94.9(4) . . . . ? B9 B1 B2 S6 63.5(4) . . . . ? S4 B1 B2 S6 0.2(5) . . . . ? Ru5 B1 B2 S6 -45.1(3) . . . . ? B3 B1 B2 Ru5 140.0(3) . . . . ? B9 B1 B2 Ru5 108.5(3) . . . . ? S4 B1 B2 Ru5 45.3(3) . . . . ? B7 S6 B2 B3 -28.8(3) . . . . ? Ru5 S6 B2 B3 107.8(3) . . . . ? B7 S6 B2 B1 -92.6(4) . . . . ? Ru5 S6 B2 B1 44.1(3) . . . . ? Ru5 S6 B2 B7 136.7(3) . . . . ? B7 S6 B2 Ru5 -136.7(3) . . . . ? C3 Ru5 B2 B3 144.6(3) . . . . ? C5 Ru5 B2 B3 88.8(4) . . . . ? C2 Ru5 B2 B3 -178.2(3) . . . . ? C4 Ru5 B2 B3 110.1(3) . . . . ? C1 Ru5 B2 B3 -150.2(3) . . . . ? B1 Ru5 B2 B3 36.6(3) . . . . ? S4 Ru5 B2 B3 5.7(3) . . . . ? S6 Ru5 B2 B3 -101.3(3) . . . . ? C3 Ru5 B2 B1 108.0(2) . . . . ? C5 Ru5 B2 B1 52.2(4) . . . . ? C2 Ru5 B2 B1 145.2(2) . . . . ? C4 Ru5 B2 B1 73.6(3) . . . . ? C1 Ru5 B2 B1 173.2(2) . . . . ? S4 Ru5 B2 B1 -30.9(2) . . . . ? S6 Ru5 B2 B1 -137.9(3) . . . . ? C3 Ru5 B2 B7 -154.2(3) . . . . ? C5 Ru5 B2 B7 150.0(3) . . . . ? C2 Ru5 B2 B7 -116.9(3) . . . . ? C4 Ru5 B2 B7 171.4(3) . . . . ? C1 Ru5 B2 B7 -89.0(4) . . . . ? B1 Ru5 B2 B7 97.8(4) . . . . ? S4 Ru5 B2 B7 66.9(3) . . . . ? S6 Ru5 B2 B7 -40.1(3) . . . . ? C3 Ru5 B2 S6 -114.12(17) . . . . ? C5 Ru5 B2 S6 -169.9(3) . . . . ? C2 Ru5 B2 S6 -76.88(19) . . . . ? C4 Ru5 B2 S6 -148.57(16) . . . . ? C1 Ru5 B2 S6 -48.9(3) . . . . ? B1 Ru5 B2 S6 137.9(3) . . . . ? S4 Ru5 B2 S6 107.00(13) . . . . ? B1 B2 B3 B7 142.9(4) . . . . ? S6 B2 B3 B7 30.1(3) . . . . ? Ru5 B2 B3 B7 103.5(3) . . . . ? B1 B2 B3 B9 37.3(4) . . . . ? B7 B2 B3 B9 -105.6(4) . . . . ? S6 B2 B3 B9 -75.5(4) . . . . ? Ru5 B2 B3 B9 -2.1(5) . . . . ? B1 B2 B3 B8 104.5(4) . . . . ? B7 B2 B3 B8 -38.5(4) . . . . ? S6 B2 B3 B8 -8.3(5) . . . . ? Ru5 B2 B3 B8 65.0(4) . . . . ? B7 B2 B3 B1 -142.9(4) . . . . ? S6 B2 B3 B1 -112.8(3) . . . . ? Ru5 B2 B3 B1 -39.5(3) . . . . ? B2 B1 B3 B7 -37.7(4) . . . . ? B9 B1 B3 B7 105.4(4) . . . . ? S4 B1 B3 B7 74.9(4) . . . . ? Ru5 B1 B3 B7 2.2(5) . . . . ? B2 B1 B3 B9 -143.1(3) . . . . ? S4 B1 B3 B9 -30.5(3) . . . . ? Ru5 B1 B3 B9 -103.3(3) . . . . ? B2 B1 B3 B8 -106.3(4) . . . . ? B9 B1 B3 B8 36.8(3) . . . . ? S4 B1 B3 B8 6.3(5) . . . . ? Ru5 B1 B3 B8 -66.4(4) . . . . ? B9 B1 B3 B2 143.1(3) . . . . ? S4 B1 B3 B2 112.6(3) . . . . ? Ru5 B1 B3 B2 39.9(3) . . . . ? B9 B3 B7 B8 -30.5(4) . . . . ? B2 B3 B7 B8 -139.8(3) . . . . ? B1 B3 B7 B8 -103.1(4) . . . . ? B9 B3 B7 B2 109.3(4) . . . . ? B8 B3 B7 B2 139.8(3) . . . . ? B1 B3 B7 B2 36.7(4) . . . . ? B9 B3 B7 S6 78.0(4) . . . . ? B8 B3 B7 S6 108.5(4) . . . . ? B2 B3 B7 S6 -31.4(3) . . . . ? B1 B3 B7 S6 5.3(5) . . . . ? B1 B2 B7 B3 -32.4(3) . . . . ? S6 B2 B7 B3 -146.4(3) . . . . ? Ru5 B2 B7 B3 -102.6(3) . . . . ? B3 B2 B7 B8 36.1(3) . . . . ? B1 B2 B7 B8 3.7(5) . . . . ? S6 B2 B7 B8 -110.3(4) . . . . ? Ru5 B2 B7 B8 -66.4(4) . . . . ? B3 B2 B7 S6 146.4(3) . . . . ? B1 B2 B7 S6 114.0(3) . . . . ? Ru5 B2 B7 S6 43.9(2) . . . . ? B2 S6 B7 B3 30.7(3) . . . . ? Ru5 S6 B7 B3 -10.0(4) . . . . ? B2 S6 B7 B8 97.2(4) . . . . ? Ru5 S6 B7 B8 56.5(4) . . . . ? Ru5 S6 B7 B2 -40.7(2) . . . . ? B7 B3 B8 B9 -147.6(4) . . . . ? B2 B3 B8 B9 -107.7(4) . . . . ? B1 B3 B8 B9 -38.8(4) . . . . ? B9 B3 B8 B7 147.6(4) . . . . ? B2 B3 B8 B7 39.9(4) . . . . ? B1 B3 B8 B7 108.9(4) . . . . ? B7 B3 B8 P1 108.8(4) . . . . ? B9 B3 B8 P1 -103.6(4) . . . . ? B2 B3 B8 P1 148.7(3) . . . . ? B1 B3 B8 P1 -142.3(3) . . . . ? B3 B7 B8 B9 29.4(3) . . . . ? B2 B7 B8 B9 -6.1(5) . . . . ? S6 B7 B8 B9 -72.0(4) . . . . ? B2 B7 B8 B3 -35.6(3) . . . . ? S6 B7 B8 B3 -101.4(4) . . . . ? B3 B7 B8 P1 -103.2(4) . . . . ? B2 B7 B8 P1 -138.7(3) . . . . ? S6 B7 B8 P1 155.5(3) . . . . ? C21 P1 B8 B9 -175.9(3) . . . . ? C31 P1 B8 B9 -53.8(4) . . . . ? C11 P1 B8 B9 64.5(4) . . . . ? C21 P1 B8 B3 -110.3(4) . . . . ? C31 P1 B8 B3 11.8(5) . . . . ? C11 P1 B8 B3 130.1(3) . . . . ? C21 P1 B8 B7 -44.7(4) . . . . ? C31 P1 B8 B7 77.4(4) . . . . ? C11 P1 B8 B7 -164.3(3) . . . . ? B7 B3 B9 B8 31.0(4) . . . . ? B2 B3 B9 B8 104.0(4) . . . . ? B1 B3 B9 B8 140.5(4) . . . . ? B7 B3 B9 S4 -77.0(4) . . . . ? B8 B3 B9 S4 -108.0(3) . . . . ? B2 B3 B9 S4 -4.0(5) . . . . ? B1 B3 B9 S4 32.4(3) . . . . ? B7 B3 B9 B1 -109.4(4) . . . . ? B8 B3 B9 B1 -140.5(4) . . . . ? B2 B3 B9 B1 -36.5(3) . . . . ? B7 B8 B9 B3 -29.0(3) . . . . ? P1 B8 B9 B3 105.9(3) . . . . ? B3 B8 B9 S4 102.0(4) . . . . ? B7 B8 B9 S4 73.0(4) . . . . ? P1 B8 B9 S4 -152.1(3) . . . . ? B3 B8 B9 B1 35.0(3) . . . . ? B7 B8 B9 B1 6.0(5) . . . . ? P1 B8 B9 B1 140.9(3) . . . . ? B1 S4 B9 B3 -31.3(3) . . . . ? Ru5 S4 B9 B3 8.1(4) . . . . ? B1 S4 B9 B8 -98.3(4) . . . . ? Ru5 S4 B9 B8 -58.9(4) . . . . ? Ru5 S4 B9 B1 39.4(2) . . . . ? B2 B1 B9 B3 32.4(3) . . . . ? S4 B1 B9 B3 145.7(3) . . . . ? Ru5 B1 B9 B3 103.3(3) . . . . ? B3 B1 B9 B8 -35.9(3) . . . . ? B2 B1 B9 B8 -3.5(4) . . . . ? S4 B1 B9 B8 109.8(3) . . . . ? Ru5 B1 B9 B8 67.5(4) . . . . ? B3 B1 B9 S4 -145.7(3) . . . . ? B2 B1 B9 S4 -113.3(3) . . . . ? Ru5 B1 B9 S4 -42.3(2) . . . . ? C3 Ru5 C1 C6 -102.3(3) . . . . ? C5 Ru5 C1 C6 -28.7(3) . . . . ? C2 Ru5 C1 C6 -130.8(4) . . . . ? C4 Ru5 C1 C6 -65.2(3) . . . . ? B2 Ru5 C1 C6 -179.0(3) . . . . ? S4 Ru5 C1 C6 34.7(4) . . . . ? S6 Ru5 C1 C6 146.5(3) . . . . ? C3 Ru5 C1 C2 28.5(3) . . . . ? C5 Ru5 C1 C2 102.0(3) . . . . ? C6 Ru5 C1 C2 130.8(4) . . . . ? C4 Ru5 C1 C2 65.5(3) . . . . ? B2 Ru5 C1 C2 -48.3(4) . . . . ? S4 Ru5 C1 C2 165.5(2) . . . . ? S6 Ru5 C1 C2 -82.8(3) . . . . ? C3 Ru5 C1 C7 139.4(6) . . . . ? C5 Ru5 C1 C7 -147.0(6) . . . . ? C2 Ru5 C1 C7 111.0(7) . . . . ? C6 Ru5 C1 C7 -118.3(7) . . . . ? C4 Ru5 C1 C7 176.5(6) . . . . ? B2 Ru5 C1 C7 62.7(6) . . . . ? S4 Ru5 C1 C7 -83.6(6) . . . . ? S6 Ru5 C1 C7 28.2(6) . . . . ? C6 C1 C2 C3 0.5(7) . . . . ? C7 C1 C2 C3 -179.4(4) . . . . ? Ru5 C1 C2 C3 -53.3(4) . . . . ? C6 C1 C2 Ru5 53.8(4) . . . . ? C7 C1 C2 Ru5 -126.1(4) . . . . ? C5 Ru5 C2 C3 66.9(3) . . . . ? C6 Ru5 C2 C3 104.0(3) . . . . ? C4 Ru5 C2 C3 29.7(3) . . . . ? C1 Ru5 C2 C3 133.6(4) . . . . ? B1 Ru5 C2 C3 -39.9(4) . . . . ? B2 Ru5 C2 C3 -80.3(3) . . . . ? S4 Ru5 C2 C3 83.3(6) . . . . ? S6 Ru5 C2 C3 -127.0(3) . . . . ? C3 Ru5 C2 C1 -133.6(4) . . . . ? C5 Ru5 C2 C1 -66.7(3) . . . . ? C6 Ru5 C2 C1 -29.6(3) . . . . ? C4 Ru5 C2 C1 -103.9(3) . . . . ? B1 Ru5 C2 C1 -173.5(3) . . . . ? B2 Ru5 C2 C1 146.1(3) . . . . ? S4 Ru5 C2 C1 -50.3(7) . . . . ? S6 Ru5 C2 C1 99.4(3) . . . . ? C1 C2 C3 C4 -2.0(7) . . . . ? Ru5 C2 C3 C4 -56.3(4) . . . . ? C1 C2 C3 Ru5 54.3(4) . . . . ? C5 Ru5 C3 C2 -101.7(3) . . . . ? C6 Ru5 C3 C2 -64.7(3) . . . . ? C4 Ru5 C3 C2 -131.3(4) . . . . ? C1 Ru5 C3 C2 -28.3(3) . . . . ? B1 Ru5 C3 C2 154.2(3) . . . . ? B2 Ru5 C3 C2 106.8(3) . . . . ? S4 Ru5 C3 C2 -158.8(2) . . . . ? S6 Ru5 C3 C2 59.5(3) . . . . ? C5 Ru5 C3 C4 29.6(3) . . . . ? C2 Ru5 C3 C4 131.3(4) . . . . ? C6 Ru5 C3 C4 66.6(3) . . . . ? C1 Ru5 C3 C4 103.0(3) . . . . ? B1 Ru5 C3 C4 -74.5(3) . . . . ? B2 Ru5 C3 C4 -121.9(3) . . . . ? S4 Ru5 C3 C4 -27.5(4) . . . . ? S6 Ru5 C3 C4 -169.2(2) . . . . ? C2 C3 C4 C5 2.7(6) . . . . ? Ru5 C3 C4 C5 -53.1(4) . . . . ? C2 C3 C4 C10 -178.7(4) . . . . ? Ru5 C3 C4 C10 125.4(4) . . . . ? C2 C3 C4 Ru5 55.9(4) . . . . ? C3 Ru5 C4 C5 131.3(4) . . . . ? C2 Ru5 C4 C5 101.6(3) . . . . ? C6 Ru5 C4 C5 28.9(3) . . . . ? C1 Ru5 C4 C5 64.9(3) . . . . ? B1 Ru5 C4 C5 -116.1(3) . . . . ? B2 Ru5 C4 C5 -161.4(3) . . . . ? S4 Ru5 C4 C5 -67.0(3) . . . . ? S6 Ru5 C4 C5 150.6(2) . . . . ? C5 Ru5 C4 C3 -131.3(4) . . . . ? C2 Ru5 C4 C3 -29.8(3) . . . . ? C6 Ru5 C4 C3 -102.4(3) . . . . ? C1 Ru5 C4 C3 -66.4(3) . . . . ? B1 Ru5 C4 C3 112.6(3) . . . . ? B2 Ru5 C4 C3 67.3(3) . . . . ? S4 Ru5 C4 C3 161.7(2) . . . . ? S6 Ru5 C4 C3 19.3(4) . . . . ? C3 Ru5 C4 C10 -113.5(5) . . . . ? C5 Ru5 C4 C10 115.2(6) . . . . ? C2 Ru5 C4 C10 -143.2(5) . . . . ? C6 Ru5 C4 C10 144.1(5) . . . . ? C1 Ru5 C4 C10 -179.9(5) . . . . ? B1 Ru5 C4 C10 -0.9(5) . . . . ? B2 Ru5 C4 C10 -46.2(5) . . . . ? S4 Ru5 C4 C10 48.2(4) . . . . ? S6 Ru5 C4 C10 -94.2(5) . . . . ? C3 C4 C5 C6 -2.2(7) . . . . ? C10 C4 C5 C6 179.3(4) . . . . ? Ru5 C4 C5 C6 -55.0(4) . . . . ? C3 C4 C5 Ru5 52.8(4) . . . . ? C10 C4 C5 Ru5 -125.7(4) . . . . ? C3 Ru5 C5 C4 -29.8(3) . . . . ? C2 Ru5 C5 C4 -67.3(3) . . . . ? C6 Ru5 C5 C4 -132.6(4) . . . . ? C1 Ru5 C5 C4 -104.5(3) . . . . ? B1 Ru5 C5 C4 71.5(3) . . . . ? B2 Ru5 C5 C4 33.3(5) . . . . ? S4 Ru5 C5 C4 116.6(3) . . . . ? S6 Ru5 C5 C4 -120.7(4) . . . . ? C3 Ru5 C5 C6 102.9(3) . . . . ? C2 Ru5 C5 C6 65.3(3) . . . . ? C4 Ru5 C5 C6 132.6(4) . . . . ? C1 Ru5 C5 C6 28.2(3) . . . . ? B1 Ru5 C5 C6 -155.8(3) . . . . ? B2 Ru5 C5 C6 166.0(3) . . . . ? S4 Ru5 C5 C6 -110.8(3) . . . . ? S6 Ru5 C5 C6 12.0(6) . . . . ? C2 C1 C6 C5 0.0(7) . . . . ? C7 C1 C6 C5 180.0(5) . . . . ? Ru5 C1 C6 C5 53.4(4) . . . . ? C2 C1 C6 Ru5 -53.3(4) . . . . ? C7 C1 C6 Ru5 126.6(5) . . . . ? C4 C5 C6 C1 0.8(7) . . . . ? Ru5 C5 C6 C1 -54.3(4) . . . . ? C4 C5 C6 Ru5 55.1(4) . . . . ? C3 Ru5 C6 C1 67.2(3) . . . . ? C5 Ru5 C6 C1 133.2(5) . . . . ? C2 Ru5 C6 C1 30.1(3) . . . . ? C4 Ru5 C6 C1 104.4(3) . . . . ? B1 Ru5 C6 C1 171.9(3) . . . . ? S4 Ru5 C6 C1 -154.8(3) . . . . ? S6 Ru5 C6 C1 -42.4(3) . . . . ? C3 Ru5 C6 C5 -66.1(3) . . . . ? C2 Ru5 C6 C5 -103.1(3) . . . . ? C4 Ru5 C6 C5 -28.8(3) . . . . ? C1 Ru5 C6 C5 -133.2(5) . . . . ? B1 Ru5 C6 C5 38.7(4) . . . . ? S4 Ru5 C6 C5 71.9(3) . . . . ? S6 Ru5 C6 C5 -175.6(2) . . . . ? C6 C1 C7 C8 -25.4(8) . . . . ? C2 C1 C7 C8 154.6(6) . . . . ? Ru5 C1 C7 C8 67.5(8) . . . . ? C6 C1 C7 C9 101.7(7) . . . . ? C2 C1 C7 C9 -78.4(7) . . . . ? Ru5 C1 C7 C9 -165.5(6) . . . . ? C21 P1 C11 C16 60.2(5) . . . . ? C31 P1 C11 C16 -52.1(5) . . . . ? B8 P1 C11 C16 -176.6(4) . . . . ? C21 P1 C11 C12 -126.3(4) . . . . ? C31 P1 C11 C12 121.4(5) . . . . ? B8 P1 C11 C12 -3.1(5) . . . . ? C16 C11 C12 C13 -1.3(9) . . . . ? P1 C11 C12 C13 -175.0(5) . . . . ? C11 C12 C13 C14 -1.4(10) . . . . ? C12 C13 C14 C15 4.2(10) . . . . ? C13 C14 C15 C16 -4.3(10) . . . . ? C12 C11 C16 C15 1.3(9) . . . . ? P1 C11 C16 C15 174.9(5) . . . . ? C14 C15 C16 C11 1.5(10) . . . . ? C31 P1 C21 C26 -19.3(5) . . . . ? C11 P1 C21 C26 -130.4(4) . . . . ? B8 P1 C21 C26 107.5(4) . . . . ? C31 P1 C21 C22 165.4(5) . . . . ? C11 P1 C21 C22 54.3(6) . . . . ? B8 P1 C21 C22 -67.8(6) . . . . ? C26 C21 C22 C23 -0.9(10) . . . . ? P1 C21 C22 C23 174.5(6) . . . . ? C21 C22 C23 C24 0.7(13) . . . . ? C22 C23 C24 C25 0.3(13) . . . . ? C23 C24 C25 C26 -1.3(10) . . . . ? C22 C21 C26 C25 0.0(8) . . . . ? P1 C21 C26 C25 -175.3(4) . . . . ? C24 C25 C26 C21 1.1(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.604 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.136 #================================================================= #==================================================================== # END of CIF for compound 4 #==================================================================== # END of CIF #====================================================================