# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1243 data_gru144 _publ_contact_author_name ; P.Bauerle ; _publ_contact_author_address ; Abteilung Organische Chemie II Universitat Ulm Albert-Einstein-Allee 11 D 89069 Ulm, Germany ; _publ_author_name ; G.Grner, T.Debaerdemaeker, P.Bauerle, ; _publ_requested_journal ; J.Chem.Soc., Chem. Commun. ; _publ_section_title ; First crystallographic structure determination of an oligothiophene metal complex ; _publ_section_exptl_refinement ; The measured intensities were corrected for Lorentz and polarization effects. The structure determination was done by direct methods. The molecule is situated on a twofold axes passing through S3 and between C23 and C23a. The positions of the hydrogen atoms were calculated (riding model) and refined isotropically. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; 5,5''-Bis{((5-cyclopentadienyl)-[(6-(4,7-di-n-butylbenzo[b]thien-2-yl)] -ruthenium}-2,2':5',2''-terthiophene bishexafluorophosphate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H58 F12 P2 Ru2 S5' _chemical_formula_weight 1359.38 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 14.4444(15) _cell_length_b 16.998(3) _cell_length_c 27.623(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.941(13) _cell_angle_gamma 90.00 _cell_volume 6680.3(16) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2 _cell_measurement_theta_max 24 _exptl_crystal_description prism _exptl_crystal_colour rubyred _exptl_crystal_size_max 0.77 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 0.721 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7754 _exptl_absorpt_correction_T_max 0.9139 _exptl_absorpt_process_details 'STOE-IPDS software' _exptl_special_details ; Although data were collected at 220K, no diffraction was observed beyond 24o. ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS, image plate' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 0.15 _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5186 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2007 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 24.04 _reflns_number_total 5186 _reflns_number_gt 1873 _reflns_threshold_expression >2sigma(I) _computing_data_collection STOE-IPDS _computing_cell_refinement STOE-IPDS _computing_data_reduction STOE-IPDS _computing_structure_solution 'XMY93 (Debaerdemaeker,1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLUTON, PLATON (Spek,1997)' _computing_publication_material 'CIFTAB (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The relatively small temperature factor for C3, compared to those from the neighbour atoms is probably due to a partial occupation of the site by sulfur, the site of S1 is probably also partially occupied by carbon, an effect which couldn't be tackled but which is also found in similar compounds by other authors. The fluorine atoms in the anion are disordered this explains their large anisotropy and the presence of the highest and lowest peak in the neighborhood of F6(1.03 A) and P1(0.66A). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1449P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5186 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1789 _refine_ls_R_factor_gt 0.0937 _refine_ls_wR_factor_ref 0.2585 _refine_ls_wR_factor_gt 0.2276 _refine_ls_goodness_of_fit_ref 0.784 _refine_ls_restrained_S_all 0.784 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.23122(8) 0.03272(7) 0.27102(4) 0.0586(4) Uani 1 d . . . S2 S -0.0366(2) 0.0153(2) 0.43257(12) 0.0620(10) Uani 1 d . . . S1 S 0.1227(3) -0.0360(3) 0.37144(15) 0.0909(13) Uani 1 d . . . S3 S -0.2500 0.1332(3) 0.5000 0.0682(15) Uani 1 d S . . C3 C 0.1905(6) 0.1237(7) 0.3806(3) 0.029(2) Uiso 1 d . . . H3 H 0.1973 0.1768 0.3887 0.035 Uiso 1 calc R . . C5 C 0.3766(10) 0.0316(11) 0.3092(5) 0.073(4) Uani 1 d . . . H5 H 0.4318 0.0448 0.2981 0.087 Uiso 1 calc R . . C8 C 0.2503(9) 0.0648(9) 0.3516(4) 0.057(4) Uani 1 d . . . C9 C 0.2203(8) -0.0150(8) 0.3458(5) 0.056(4) Uani 1 d . . . C23 C -0.2085(9) -0.0117(10) 0.4892(4) 0.065(4) Uani 1 d . . . H23 H -0.1782 -0.0572 0.4815 0.078 Uiso 1 calc R . . C21 C -0.0984(9) 0.0835(9) 0.4597(5) 0.059(4) Uani 1 d . . . C2 C 0.1157(9) 0.0589(8) 0.3907(4) 0.054(3) Uani 1 d . . . C6 C 0.3466(9) -0.0443(10) 0.3033(5) 0.065(4) Uani 1 d . . . H6 H 0.3806 -0.0801 0.2878 0.078 Uiso 1 calc R . . C4 C 0.3293(9) 0.0926(9) 0.3311(4) 0.056(3) Uani 1 d . . . C22 C -0.1783(8) 0.0636(9) 0.4812(4) 0.058(4) Uani 1 d . . . C18 C 0.0403(8) 0.0824(9) 0.4160(4) 0.058(4) Uani 1 d . . . C7 C 0.2649(10) -0.0697(9) 0.3202(5) 0.067(4) Uani 1 d . . . C20 C -0.0593(11) 0.1555(11) 0.4562(6) 0.091(5) Uani 1 d . . . H20 H -0.0823 0.2009 0.4688 0.109 Uiso 1 calc R . . C10 C 0.3598(11) 0.1753(10) 0.3363(6) 0.082(5) Uani 1 d . . . H10A H 0.3046 0.2088 0.3324 0.099 Uiso 1 calc R . . H10B H 0.3943 0.1881 0.3102 0.099 Uiso 1 calc R . . C25 C 0.1006(15) 0.0161(17) 0.2189(8) 0.108(7) Uani 1 d . . . H25 H 0.0536 -0.0183 0.2247 0.130 Uiso 1 calc R . . C19 C 0.0212(9) 0.1559(10) 0.4312(5) 0.076(5) Uani 1 d . . . H19 H 0.0553 0.2007 0.4262 0.091 Uiso 1 calc R . . C14 C 0.2282(11) -0.1562(9) 0.3118(6) 0.075(4) Uani 1 d . . . H14A H 0.1600 -0.1563 0.3059 0.090 Uiso 1 calc R . . H14B H 0.2490 -0.1779 0.2831 0.090 Uiso 1 calc R . . C27 C 0.2296(18) 0.061(3) 0.1947(8) 0.169(17) Uani 1 d . . . H27 H 0.2837 0.0638 0.1808 0.202 Uiso 1 calc R . . C15 C 0.2643(12) -0.2065(10) 0.3561(6) 0.086(5) Uani 1 d . . . H15A H 0.2492 -0.1822 0.3855 0.103 Uiso 1 calc R . . H15B H 0.3321 -0.2117 0.3600 0.103 Uiso 1 calc R . . C24 C 0.1079(18) 0.092(2) 0.2316(6) 0.115(8) Uani 1 d . . . H24 H 0.0646 0.1193 0.2467 0.138 Uiso 1 calc R . . C11 C 0.4224(11) 0.1936(9) 0.3863(5) 0.077(4) Uani 1 d . . . H11A H 0.3899 0.1788 0.4129 0.092 Uiso 1 calc R . . H11B H 0.4801 0.1634 0.3896 0.092 Uiso 1 calc R . . C12 C 0.4447(16) 0.2796(13) 0.3894(9) 0.136(8) Uani 1 d . . . H12A H 0.3871 0.3100 0.3856 0.163 Uiso 1 calc R . . H12B H 0.4784 0.2943 0.3632 0.163 Uiso 1 calc R . . C26 C 0.173(2) -0.0020(17) 0.1960(7) 0.126(10) Uani 1 d . . . H26 H 0.1834 -0.0510 0.1829 0.151 Uiso 1 calc R . . C16 C 0.2178(17) -0.2881(11) 0.3486(9) 0.128(8) Uani 1 d . . . H16A H 0.1501 -0.2823 0.3446 0.154 Uiso 1 calc R . . H16B H 0.2325 -0.3117 0.3189 0.154 Uiso 1 calc R . . C28 C 0.188(3) 0.1251(15) 0.2196(11) 0.135(10) Uani 1 d . . . H28 H 0.2110 0.1759 0.2258 0.162 Uiso 1 calc R . . C13 C 0.505(2) 0.296(2) 0.4388(10) 0.217(15) Uani 1 d . . . H13A H 0.5201 0.3513 0.4411 0.260 Uiso 1 calc R . . H13B H 0.5611 0.2658 0.4423 0.260 Uiso 1 calc R . . H13C H 0.4702 0.2827 0.4644 0.260 Uiso 1 calc R . . C17 C 0.252(2) -0.3413(14) 0.3918(9) 0.198(15) Uani 1 d . . . H17A H 0.2208 -0.3913 0.3866 0.238 Uiso 1 calc R . . H17B H 0.2375 -0.3178 0.4213 0.238 Uiso 1 calc R . . H17C H 0.3184 -0.3485 0.3950 0.238 Uiso 1 calc R . . P1 P 0.0218(4) 0.2906(4) 0.3000(2) 0.1076(17) Uiso 1 d . . . F6 F 0.0311(14) 0.3692(13) 0.2749(7) 0.231(8) Uiso 1 d . . . F4 F 0.1239(10) 0.2643(8) 0.2919(4) 0.147(4) Uiso 1 d . . . F2 F -0.0022(10) 0.2029(8) 0.3087(5) 0.150(5) Uiso 1 d . . . F1 F -0.0836(14) 0.3154(11) 0.3073(7) 0.216(7) Uiso 1 d . . . F5 F -0.0112(15) 0.2757(12) 0.2473(7) 0.220(7) Uiso 1 d . . . F3 F 0.0529(15) 0.3045(12) 0.3517(7) 0.225(8) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0458(6) 0.0796(8) 0.0543(6) 0.0035(7) 0.0199(4) 0.0040(7) S2 0.0449(19) 0.090(3) 0.0577(19) -0.0034(18) 0.0264(15) -0.0045(18) S1 0.066(2) 0.126(4) 0.088(3) 0.000(3) 0.032(2) 0.001(3) S3 0.049(3) 0.096(4) 0.068(3) 0.000 0.033(2) 0.000 C5 0.058(8) 0.100(12) 0.064(8) -0.005(10) 0.022(7) 0.000(10) C8 0.043(8) 0.084(10) 0.047(7) 0.002(7) 0.014(6) 0.009(7) C9 0.027(6) 0.076(11) 0.066(8) 0.007(7) 0.012(6) 0.001(6) C23 0.046(8) 0.104(13) 0.053(7) -0.005(8) 0.028(6) -0.002(8) C21 0.047(8) 0.079(10) 0.058(8) -0.004(7) 0.027(6) 0.002(7) C2 0.044(7) 0.069(10) 0.053(7) 0.000(6) 0.017(6) -0.004(6) C6 0.047(8) 0.077(12) 0.075(9) -0.009(8) 0.023(7) 0.015(8) C4 0.044(8) 0.078(10) 0.049(7) -0.004(7) 0.017(6) 0.000(7) C22 0.034(7) 0.104(12) 0.040(7) -0.007(7) 0.017(5) 0.004(7) C18 0.039(7) 0.088(11) 0.054(7) -0.008(7) 0.026(6) -0.006(7) C7 0.058(9) 0.084(11) 0.064(9) 0.007(8) 0.023(7) 0.016(8) C20 0.072(11) 0.103(14) 0.113(13) 0.001(11) 0.059(10) 0.012(10) C10 0.068(10) 0.104(14) 0.085(11) 0.005(10) 0.041(9) 0.006(9) C25 0.085(15) 0.13(2) 0.093(15) 0.023(14) -0.036(12) -0.033(14) C19 0.046(9) 0.107(13) 0.084(10) 0.001(9) 0.038(8) -0.011(8) C14 0.072(10) 0.069(11) 0.078(10) 0.016(8) -0.004(8) -0.007(8) C27 0.093(17) 0.35(5) 0.056(12) 0.06(2) 0.001(11) -0.06(3) C15 0.087(12) 0.102(14) 0.073(10) 0.006(10) 0.029(9) 0.020(10) C24 0.110(19) 0.17(3) 0.060(11) 0.010(15) -0.012(11) 0.046(18) C11 0.072(11) 0.079(11) 0.076(10) -0.022(9) 0.007(8) -0.005(9) C12 0.116(18) 0.112(18) 0.16(2) -0.005(16) -0.023(16) -0.026(14) C26 0.14(2) 0.18(3) 0.054(11) -0.039(13) -0.008(13) 0.060(19) C16 0.17(2) 0.064(12) 0.17(2) 0.006(13) 0.077(18) 0.008(13) C28 0.15(3) 0.113(19) 0.12(2) 0.029(15) -0.033(18) -0.043(19) C13 0.25(4) 0.22(3) 0.16(3) 0.01(2) -0.04(3) -0.02(3) C17 0.36(5) 0.12(2) 0.15(2) 0.043(17) 0.15(3) 0.03(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 C28 2.14(2) . ? Ru1 C27 2.159(19) . ? Ru1 C24 2.170(19) . ? Ru1 C26 2.178(18) . ? Ru1 C5 2.181(14) . ? Ru1 C6 2.185(13) . ? Ru1 C25 2.186(17) . ? Ru1 C7 2.210(14) . ? Ru1 C4 2.232(13) . ? Ru1 C9 2.251(13) . ? Ru1 C8 2.263(12) . ? S2 C18 1.709(13) . ? S2 C21 1.714(13) . ? S1 C2 1.706(14) . ? S1 C9 1.720(12) . ? S3 C22 1.711(13) 2_456 ? S3 C22 1.711(13) . ? C3 C2 1.600(15) . ? C3 C8 1.621(15) . ? C5 C6 1.36(2) . ? C5 C4 1.432(19) . ? C8 C9 1.425(18) . ? C8 C4 1.438(17) . ? C9 C7 1.392(18) . ? C23 C22 1.383(19) . ? C23 C23 1.43(2) 2_456 ? C21 C20 1.36(2) . ? C21 C22 1.427(17) . ? C2 C18 1.449(16) . ? C6 C7 1.410(18) . ? C4 C10 1.47(2) . ? C18 C19 1.363(19) . ? C7 C14 1.57(2) . ? C20 C19 1.451(18) . ? C10 C11 1.55(2) . ? C25 C24 1.34(3) . ? C25 C26 1.35(3) . ? C14 C15 1.51(2) . ? C27 C26 1.35(3) . ? C27 C28 1.46(4) . ? C15 C16 1.54(2) . ? C24 C28 1.38(3) . ? C11 C12 1.50(2) . ? C12 C13 1.51(3) . ? C16 C17 1.51(3) . ? P1 F3 1.439(19) . ? P1 F5 1.47(2) . ? P1 F6 1.52(2) . ? P1 F2 1.559(15) . ? P1 F4 1.594(14) . ? P1 F1 1.63(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C28 Ru1 C27 39.9(11) . . ? C28 Ru1 C24 37.4(9) . . ? C27 Ru1 C24 62.4(10) . . ? C28 Ru1 C26 63.0(10) . . ? C27 Ru1 C26 36.3(9) . . ? C24 Ru1 C26 60.2(8) . . ? C28 Ru1 C5 118.2(10) . . ? C27 Ru1 C5 108.7(8) . . ? C24 Ru1 C5 152.2(11) . . ? C26 Ru1 C5 129.5(9) . . ? C28 Ru1 C6 145.6(12) . . ? C27 Ru1 C6 114.3(11) . . ? C24 Ru1 C6 170.4(10) . . ? C26 Ru1 C6 111.5(7) . . ? C5 Ru1 C6 36.4(5) . . ? C28 Ru1 C25 62.5(8) . . ? C27 Ru1 C25 61.5(9) . . ? C24 Ru1 C25 35.8(8) . . ? C26 Ru1 C25 36.1(8) . . ? C5 Ru1 C25 165.3(10) . . ? C6 Ru1 C25 134.6(9) . . ? C28 Ru1 C7 174.6(8) . . ? C27 Ru1 C7 137.9(15) . . ? C24 Ru1 C7 138.5(10) . . ? C26 Ru1 C7 112.3(9) . . ? C5 Ru1 C7 66.7(6) . . ? C6 Ru1 C7 37.4(5) . . ? C25 Ru1 C7 112.1(7) . . ? C28 Ru1 C4 103.5(8) . . ? C27 Ru1 C4 121.5(11) . . ? C24 Ru1 C4 121.4(9) . . ? C26 Ru1 C4 157.0(11) . . ? C5 Ru1 C4 37.8(5) . . ? C6 Ru1 C4 68.2(5) . . ? C25 Ru1 C4 156.0(9) . . ? C7 Ru1 C4 81.8(5) . . ? C28 Ru1 C9 144.8(12) . . ? C27 Ru1 C9 170.6(13) . . ? C24 Ru1 C9 116.5(7) . . ? C26 Ru1 C9 134.4(11) . . ? C5 Ru1 C9 76.6(5) . . ? C6 Ru1 C9 65.1(5) . . ? C25 Ru1 C9 111.7(7) . . ? C7 Ru1 C9 36.3(5) . . ? C4 Ru1 C9 67.5(5) . . ? C28 Ru1 C8 116.7(10) . . ? C27 Ru1 C8 152.3(15) . . ? C24 Ru1 C8 109.3(7) . . ? C26 Ru1 C8 164.4(10) . . ? C5 Ru1 C8 65.4(5) . . ? C6 Ru1 C8 77.8(5) . . ? C25 Ru1 C8 128.6(9) . . ? C7 Ru1 C8 66.9(5) . . ? C4 Ru1 C8 37.3(4) . . ? C9 Ru1 C8 36.8(5) . . ? C18 S2 C21 94.4(7) . . ? C2 S1 C9 91.6(7) . . ? C22 S3 C22 92.5(10) 2_456 . ? C2 C3 C8 95.4(9) . . ? C6 C5 C4 124.8(13) . . ? C6 C5 Ru1 72.0(8) . . ? C4 C5 Ru1 73.0(8) . . ? C9 C8 C4 120.9(12) . . ? C9 C8 C3 117.8(11) . . ? C4 C8 C3 121.3(12) . . ? C9 C8 Ru1 71.1(8) . . ? C4 C8 Ru1 70.2(7) . . ? C3 C8 Ru1 130.6(8) . . ? C7 C9 C8 122.3(12) . . ? C7 C9 S1 123.7(11) . . ? C8 C9 S1 114.0(10) . . ? C7 C9 Ru1 70.3(8) . . ? C8 C9 Ru1 72.1(7) . . ? S1 C9 Ru1 130.2(7) . . ? C22 C23 C23 112.2(7) . 2_456 ? C20 C21 C22 128.3(13) . . ? C20 C21 S2 109.0(10) . . ? C22 C21 S2 122.7(12) . . ? C18 C2 C3 118.7(11) . . ? C18 C2 S1 120.0(10) . . ? C3 C2 S1 121.3(8) . . ? C5 C6 C7 121.1(13) . . ? C5 C6 Ru1 71.6(9) . . ? C7 C6 Ru1 72.3(8) . . ? C5 C4 C8 113.5(13) . . ? C5 C4 C10 125.1(13) . . ? C8 C4 C10 121.2(12) . . ? C5 C4 Ru1 69.1(8) . . ? C8 C4 Ru1 72.5(8) . . ? C10 C4 Ru1 130.4(10) . . ? C23 C22 C21 125.9(12) . . ? C23 C22 S3 111.6(9) . . ? C21 C22 S3 122.5(12) . . ? C19 C18 C2 127.7(12) . . ? C19 C18 S2 110.7(9) . . ? C2 C18 S2 121.6(11) . . ? C9 C7 C6 116.9(14) . . ? C9 C7 C14 121.9(13) . . ? C6 C7 C14 121.2(13) . . ? C9 C7 Ru1 73.4(8) . . ? C6 C7 Ru1 70.3(8) . . ? C14 C7 Ru1 127.9(10) . . ? C21 C20 C19 114.5(15) . . ? C4 C10 C11 113.4(13) . . ? C24 C25 C26 108(2) . . ? C24 C25 Ru1 71.4(11) . . ? C26 C25 Ru1 71.6(11) . . ? C18 C19 C20 111.4(14) . . ? C15 C14 C7 110.5(13) . . ? C26 C27 C28 106(2) . . ? C26 C27 Ru1 72.6(12) . . ? C28 C27 Ru1 69.2(12) . . ? C14 C15 C16 108.6(15) . . ? C25 C24 C28 111(2) . . ? C25 C24 Ru1 72.7(12) . . ? C28 C24 Ru1 70.0(13) . . ? C12 C11 C10 109.4(15) . . ? C11 C12 C13 109(2) . . ? C27 C26 C25 110(2) . . ? C27 C26 Ru1 71.1(13) . . ? C25 C26 Ru1 72.2(10) . . ? C17 C16 C15 111(2) . . ? C24 C28 C27 104(2) . . ? C24 C28 Ru1 72.6(13) . . ? C27 C28 Ru1 70.9(14) . . ? F3 P1 F5 179.2(12) . . ? F3 P1 F6 105.8(12) . . ? F5 P1 F6 74.8(10) . . ? F3 P1 F2 92.5(10) . . ? F5 P1 F2 86.9(10) . . ? F6 P1 F2 161.6(10) . . ? F3 P1 F4 92.7(10) . . ? F5 P1 F4 87.8(10) . . ? F6 P1 F4 91.4(10) . . ? F2 P1 F4 89.4(8) . . ? F3 P1 F1 88.5(11) . . ? F5 P1 F1 91.0(11) . . ? F6 P1 F1 89.3(11) . . ? F2 P1 F1 89.5(9) . . ? F4 P1 F1 178.4(9) . . ? _diffrn_measured_fraction_theta_max 0.473 _diffrn_reflns_theta_full 24.04 _diffrn_measured_fraction_theta_full 0.473 _refine_diff_density_max '1.55, 1.03 \%A from F6' _refine_diff_density_min -1.304 _refine_diff_density_rms 0.148