# ja012472z.cif data_2b _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,3-bis(2,3,4,5,1',2',3',4'-octamethylferrocen-1-yl)allylium hexafluorophosphate ; _chemical_name_common '2b, [Fc"(CH)3Fc"]+[PF6]-' _chemical_formula_moiety 'C39 H53 F6 Fe2 P' _chemical_formula_sum 'C39 H53 F6 Fe2 P' _chemical_formula_weight 778.48 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.446(3) _cell_length_b 17.746(5) _cell_length_c 21.634(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3626.5(19) _cell_formula_units_Z 4 _cell_measurement_temperature 85 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17.5 _cell_measurement_theta_max 17.8 _exptl_crystal_description Green _exptl_crystal_colour Blades _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 0.902 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 85 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD-4' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 75 _diffrn_standards_decay_% 'Within counting statistics, zero' _diffrn_reflns_number 11341 _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.9 _diffrn_reflns_theta_max 25.0 _reflns_number_total 6354 _reflns_number_gt 5999 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'CRYM (Duchamp, 1964)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme 'Observed' _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'All havy atoms in direct methods solution' _atom_sites_solution_hydrogens 'Difference Fourier map' _refine_ls_hydrogen_treatment 'Unrestrained' _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 -0.010(12) _refine_ls_number_reflns 6354 _refine_ls_number_parameters 645 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0587 _refine_ls_goodness_of_fit_ref 1.507 _refine_ls_restrained_S_all 1.507 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.94848(4) 0.28823(2) 0.739278(16) 0.01126(9) Uani 1 1 d . . . Fe2 Fe 0.38943(4) 0.48356(2) 0.952725(16) 0.01063(9) Uani 1 1 d . . . P P -0.01848(8) 0.44670(4) 1.15548(3) 0.01982(17) Uani 1 1 d . . . F1 F 0.00605(18) 0.48515(10) 1.08941(7) 0.0332(4) Uani 1 1 d . . . F2 F -0.0429(2) 0.40941(11) 1.22190(8) 0.0453(5) Uani 1 1 d . . . F3 F -0.1816(2) 0.46527(17) 1.15217(11) 0.0702(8) Uani 1 1 d . . . F4 F 0.1448(2) 0.43120(18) 1.15973(12) 0.0886(11) Uani 1 1 d . . . F5 F 0.0038(3) 0.52563(12) 1.18773(9) 0.0683(8) Uani 1 1 d . . . F6 F -0.0438(4) 0.36917(12) 1.12361(11) 0.0852(10) Uani 1 1 d . . . C1 C 0.9166(3) 0.38130(13) 0.79407(11) 0.0112(6) Uani 1 1 d . . . C2 C 0.9714(3) 0.31796(14) 0.82945(11) 0.0131(6) Uani 1 1 d . . . C3 C 1.1067(3) 0.29944(14) 0.80544(11) 0.0135(5) Uani 1 1 d . . . C4 C 1.1348(3) 0.34807(14) 0.75376(12) 0.0134(6) Uani 1 1 d . . . C5 C 1.0182(3) 0.39686(13) 0.74548(12) 0.0120(5) Uani 1 1 d . . . C6 C 0.8579(3) 0.18322(14) 0.73750(14) 0.0175(6) Uani 1 1 d . . . C7 C 0.9828(3) 0.18364(14) 0.70103(12) 0.0148(6) Uani 1 1 d . . . C8 C 0.9633(3) 0.23848(14) 0.65309(12) 0.0161(6) Uani 1 1 d . . . C9 C 0.8264(3) 0.27167(15) 0.66112(13) 0.0170(6) Uani 1 1 d . . . C10 C 0.7615(3) 0.23664(15) 0.71342(13) 0.0183(6) Uani 1 1 d . . . C11 C 0.9060(3) 0.28078(16) 0.88544(13) 0.0169(6) Uani 1 1 d . . . C12 C 1.2062(3) 0.24147(17) 0.83024(15) 0.0180(6) Uani 1 1 d . . . C13 C 1.2690(3) 0.34777(18) 0.71657(14) 0.0196(6) Uani 1 1 d . . . C14 C 1.0054(3) 0.45765(16) 0.69771(13) 0.0166(6) Uani 1 1 d . . . C15 C 1.1081(4) 0.13258(17) 0.70792(15) 0.0234(7) Uani 1 1 d . . . C16 C 1.0657(4) 0.25552(19) 0.60189(14) 0.0253(7) Uani 1 1 d . . . C17 C 0.7611(4) 0.33005(19) 0.61977(16) 0.0295(8) Uani 1 1 d . . . C18 C 0.6160(3) 0.2517(2) 0.73760(18) 0.0301(7) Uani 1 1 d . . . C21 C 0.4217(3) 0.42571(13) 0.87133(11) 0.0115(6) Uani 1 1 d . . . C22 C 0.4010(3) 0.37402(13) 0.92295(11) 0.0112(5) Uani 1 1 d . . . C23 C 0.2638(3) 0.38803(14) 0.94733(12) 0.0114(5) Uani 1 1 d . . . C24 C 0.2000(3) 0.44839(14) 0.91353(12) 0.0114(5) Uani 1 1 d . . . C25 C 0.2968(3) 0.47283(14) 0.86756(11) 0.0121(5) Uani 1 1 d . . . C26 C 0.3485(3) 0.52444(16) 1.03966(12) 0.0148(6) Uani 1 1 d . . . C27 C 0.3462(3) 0.58484(15) 0.99597(12) 0.0150(6) Uani 1 1 d . . . C28 C 0.4811(3) 0.58715(14) 0.96700(12) 0.0174(6) Uani 1 1 d . . . C29 C 0.5672(3) 0.52865(16) 0.99410(12) 0.0196(6) Uani 1 1 d . . . C30 C 0.4844(3) 0.49002(15) 1.03882(12) 0.0177(6) Uani 1 1 d . . . C31 C 0.4955(3) 0.31077(15) 0.94322(13) 0.0153(6) Uani 1 1 d . . . C32 C 0.1953(3) 0.34567(17) 0.99897(14) 0.0175(6) Uani 1 1 d . . . C33 C 0.0561(3) 0.48034(17) 0.92497(13) 0.0149(5) Uani 1 1 d . . . C34 C 0.2723(3) 0.53343(16) 0.82076(13) 0.0183(6) Uani 1 1 d . . . C35 C 0.2244(4) 0.63726(18) 0.98469(17) 0.0262(7) Uani 1 1 d . . . C36 C 0.5287(5) 0.64397(19) 0.92013(17) 0.0351(9) Uani 1 1 d . . . C37 C 0.7195(3) 0.5127(2) 0.97920(19) 0.0355(9) Uani 1 1 d . . . C38 C 0.5279(4) 0.42456(18) 1.07784(15) 0.0314(8) Uani 1 1 d . . . C40 C 0.7803(3) 0.41500(14) 0.79698(12) 0.0120(6) Uani 1 1 d . . . C41 C 0.6729(3) 0.40075(15) 0.83855(12) 0.0127(6) Uani 1 1 d . . . C42 C 0.5455(3) 0.43865(14) 0.83596(11) 0.0132(5) Uani 1 1 d . . . H6 H 0.842(3) 0.1517(14) 0.7715(12) 0.012(7) Uiso 1 1 d . . . H11A H 0.969(3) 0.2400(16) 0.8967(13) 0.027(8) Uiso 1 1 d . . . H11B H 0.811(3) 0.2596(16) 0.8783(13) 0.018(8) Uiso 1 1 d . . . H11C H 0.904(3) 0.3168(16) 0.9204(13) 0.027(8) Uiso 1 1 d . . . H12A H 1.275(4) 0.2274(19) 0.7972(16) 0.043(10) Uiso 1 1 d . . . H12B H 1.147(3) 0.1940(17) 0.8423(13) 0.029(9) Uiso 1 1 d . . . H12C H 1.249(3) 0.2571(18) 0.8628(16) 0.032(10) Uiso 1 1 d . . . H13A H 1.341(3) 0.3769(15) 0.7369(12) 0.015(7) Uiso 1 1 d . . . H13B H 1.303(3) 0.2952(17) 0.7064(13) 0.024(8) Uiso 1 1 d . . . H13C H 1.263(3) 0.3723(15) 0.6772(14) 0.018(8) Uiso 1 1 d . . . H14A H 1.052(3) 0.4442(16) 0.6631(14) 0.026(8) Uiso 1 1 d . . . H14B H 0.908(4) 0.4688(17) 0.6840(13) 0.032(9) Uiso 1 1 d . . . H14C H 1.055(3) 0.5039(16) 0.7124(13) 0.027(8) Uiso 1 1 d . . . H15A H 1.098(3) 0.0886(17) 0.6823(14) 0.024(8) Uiso 1 1 d . . . H15B H 1.121(4) 0.1128(17) 0.7542(16) 0.039(9) Uiso 1 1 d . . . H15C H 1.196(4) 0.1577(17) 0.6968(14) 0.025(8) Uiso 1 1 d . . . H16A H 1.056(3) 0.3039(18) 0.5876(14) 0.027(9) Uiso 1 1 d . . . H16B H 1.039(3) 0.2272(17) 0.5654(14) 0.034(9) Uiso 1 1 d . . . H16C H 1.172(4) 0.2425(16) 0.6168(14) 0.029(9) Uiso 1 1 d . . . H17A H 0.829(4) 0.362(2) 0.6001(18) 0.059(13) Uiso 1 1 d . . . H17B H 0.694(4) 0.3634(17) 0.6413(14) 0.032(9) Uiso 1 1 d . . . H17C H 0.710(4) 0.3087(17) 0.5841(15) 0.036(9) Uiso 1 1 d . . . H18A H 0.550(4) 0.2218(19) 0.7185(14) 0.035(9) Uiso 1 1 d . . . H18B H 0.591(3) 0.3024(17) 0.7288(13) 0.021(8) Uiso 1 1 d . . . H18C H 0.619(4) 0.2404(19) 0.7816(16) 0.045(11) Uiso 1 1 d . . . H26 H 0.282(3) 0.5104(15) 1.0631(12) 0.015(8) Uiso 1 1 d . . . H31A H 0.454(3) 0.2830(15) 0.9785(13) 0.018(7) Uiso 1 1 d . . . H31B H 0.495(3) 0.2748(17) 0.9114(14) 0.029(9) Uiso 1 1 d . . . H31C H 0.594(3) 0.3297(14) 0.9573(13) 0.016(7) Uiso 1 1 d . . . H32A H 0.159(3) 0.3009(18) 0.9863(13) 0.025(9) Uiso 1 1 d . . . H32B H 0.118(4) 0.3777(17) 1.0188(13) 0.030(9) Uiso 1 1 d . . . H32C H 0.259(3) 0.3303(15) 1.0303(13) 0.020(8) Uiso 1 1 d . . . H33A H 0.033(3) 0.4807(16) 0.9668(14) 0.020(7) Uiso 1 1 d . . . H33B H -0.011(3) 0.4563(16) 0.9000(14) 0.027(9) Uiso 1 1 d . . . H33C H 0.036(4) 0.5341(18) 0.9112(14) 0.034(9) Uiso 1 1 d . . . H34A H 0.352(3) 0.5618(15) 0.8120(12) 0.012(7) Uiso 1 1 d . . . H34B H 0.244(3) 0.5120(17) 0.7798(14) 0.028(8) Uiso 1 1 d . . . H34C H 0.207(4) 0.5666(18) 0.8337(15) 0.036(10) Uiso 1 1 d . . . H35A H 0.247(4) 0.6888(19) 1.0064(14) 0.042(10) Uiso 1 1 d . . . H35C H 0.140(4) 0.6128(18) 0.9994(15) 0.032(10) Uiso 1 1 d . . . H35B H 0.216(3) 0.6524(17) 0.9437(15) 0.027(9) Uiso 1 1 d . . . H36A H 0.449(4) 0.6613(19) 0.9010(16) 0.047(12) Uiso 1 1 d . . . H36B H 0.571(4) 0.690(2) 0.9389(17) 0.061(12) Uiso 1 1 d . . . H36C H 0.614(4) 0.6220(19) 0.8854(17) 0.055(11) Uiso 1 1 d . . . H37A H 0.748(4) 0.458(2) 0.9850(17) 0.065(14) Uiso 1 1 d . . . H37B H 0.737(3) 0.5321(16) 0.9360(13) 0.018(8) Uiso 1 1 d . . . H37C H 0.774(4) 0.534(2) 1.0072(16) 0.046(11) Uiso 1 1 d . . . H38A H 0.592(3) 0.4398(16) 1.1044(14) 0.023(8) Uiso 1 1 d . . . H38B H 0.583(3) 0.3880(17) 1.0575(14) 0.029(9) Uiso 1 1 d . . . H38C H 0.437(4) 0.397(2) 1.1015(18) 0.068(13) Uiso 1 1 d . . . H40 H 0.761(3) 0.4530(15) 0.7692(12) 0.015(7) Uiso 1 1 d . . . H41 H 0.690(3) 0.3644(14) 0.8647(11) 0.005(7) Uiso 1 1 d . . . H42 H 0.539(3) 0.4767(14) 0.8024(11) 0.004(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.00845(17) 0.01238(18) 0.01295(17) -0.00114(15) 0.00065(15) -0.00092(16) Fe2 0.00810(17) 0.01285(17) 0.01092(17) -0.00068(16) -0.00072(16) 0.00077(16) P 0.0147(4) 0.0245(4) 0.0202(4) -0.0029(3) 0.0029(3) -0.0038(3) F1 0.0347(10) 0.0457(10) 0.0191(8) 0.0016(8) 0.0022(8) 0.0003(10) F2 0.0564(13) 0.0454(11) 0.0340(11) 0.0113(9) 0.0146(10) -0.0060(11) F3 0.0195(11) 0.137(2) 0.0546(14) 0.0040(16) 0.0078(10) 0.0107(14) F4 0.0223(12) 0.167(3) 0.0762(18) 0.0691(19) 0.0110(12) 0.0301(15) F5 0.124(2) 0.0503(13) 0.0310(11) -0.0142(10) 0.0118(13) -0.0479(16) F6 0.151(3) 0.0412(12) 0.0632(15) -0.0296(11) 0.0668(18) -0.0439(16) C1 0.0135(14) 0.0097(12) 0.0103(12) -0.0008(10) -0.0010(11) -0.0006(11) C2 0.0142(14) 0.0133(12) 0.0118(12) -0.0037(10) -0.0020(11) -0.0008(11) C3 0.0121(12) 0.0133(13) 0.0153(12) -0.0044(11) -0.0006(12) -0.0005(12) C4 0.0102(14) 0.0140(13) 0.0159(14) -0.0035(11) -0.0020(11) -0.0024(11) C5 0.0106(13) 0.0122(12) 0.0132(12) -0.0045(10) -0.0010(11) -0.0030(10) C6 0.0211(16) 0.0124(13) 0.0191(14) -0.0035(12) 0.0034(13) -0.0078(12) C7 0.0142(14) 0.0129(13) 0.0174(13) -0.0038(11) -0.0014(12) -0.0016(11) C8 0.0177(15) 0.0170(13) 0.0136(13) -0.0073(11) 0.0024(13) -0.0021(12) C9 0.0128(14) 0.0196(15) 0.0185(14) -0.0049(12) -0.0067(12) 0.0000(12) C10 0.0108(14) 0.0187(15) 0.0253(15) -0.0142(12) 0.0012(12) -0.0053(12) C11 0.0159(15) 0.0188(14) 0.0160(14) 0.0035(12) 0.0000(12) 0.0037(14) C12 0.0137(15) 0.0175(15) 0.0229(16) -0.0011(13) -0.0061(14) 0.0037(13) C13 0.0117(15) 0.0231(16) 0.0238(16) -0.0016(14) 0.0042(13) -0.0027(13) C14 0.0148(14) 0.0196(15) 0.0155(14) 0.0006(12) 0.0039(12) -0.0018(13) C15 0.0235(17) 0.0182(15) 0.0284(17) -0.0068(13) -0.0049(16) 0.0030(15) C16 0.0250(18) 0.0325(18) 0.0183(15) -0.0025(14) 0.0066(14) -0.0046(16) C17 0.034(2) 0.0273(18) 0.0270(17) -0.0031(15) -0.0158(16) 0.0079(17) C18 0.0132(15) 0.0339(19) 0.043(2) -0.0198(18) 0.0035(17) -0.0053(15) C21 0.0135(14) 0.0110(12) 0.0099(12) -0.0040(10) 0.0004(11) 0.0015(11) C22 0.0100(13) 0.0121(12) 0.0116(12) -0.0026(10) -0.0017(11) 0.0009(11) C23 0.0090(13) 0.0130(12) 0.0121(13) -0.0020(11) 0.0001(11) -0.0043(11) C24 0.0093(13) 0.0132(12) 0.0118(13) -0.0050(11) -0.0036(11) 0.0014(11) C25 0.0123(13) 0.0136(13) 0.0102(12) -0.0014(11) -0.0036(10) 0.0018(11) C26 0.0154(14) 0.0178(14) 0.0111(13) -0.0052(12) 0.0021(11) -0.0022(12) C27 0.0153(14) 0.0132(14) 0.0166(14) -0.0077(11) -0.0037(12) 0.0010(11) C28 0.0162(15) 0.0157(13) 0.0202(14) -0.0045(12) -0.0004(12) -0.0047(12) C29 0.0107(14) 0.0254(15) 0.0226(14) -0.0149(13) -0.0041(12) -0.0023(13) C30 0.0210(15) 0.0175(13) 0.0146(13) -0.0062(12) -0.0090(12) 0.0013(12) C31 0.0138(14) 0.0164(13) 0.0157(14) 0.0008(12) 0.0006(12) 0.0021(12) C32 0.0169(16) 0.0177(15) 0.0178(15) 0.0031(13) 0.0006(13) -0.0022(13) C33 0.0082(12) 0.0220(14) 0.0145(13) -0.0028(13) -0.0029(12) 0.0022(13) C34 0.0179(15) 0.0195(16) 0.0177(15) 0.0030(13) -0.0006(13) 0.0051(14) C35 0.0251(18) 0.0211(17) 0.032(2) -0.0095(15) -0.0084(16) 0.0059(15) C36 0.046(2) 0.0264(18) 0.0328(19) 0.0013(15) 0.0053(19) -0.0144(18) C37 0.0132(16) 0.051(2) 0.043(2) -0.024(2) -0.0006(16) -0.0016(17) C38 0.048(2) 0.0239(17) 0.0219(16) -0.0071(14) -0.0182(18) 0.0123(17) C40 0.0138(14) 0.0076(12) 0.0145(13) 0.0001(11) 0.0001(12) -0.0010(11) C41 0.0144(14) 0.0139(14) 0.0097(13) 0.0010(11) -0.0007(12) 0.0031(12) C42 0.0163(13) 0.0133(13) 0.0099(12) -0.0004(11) -0.0016(12) -0.0025(12) _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 Fe1 C2 2.032(3) . yes Fe1 C5 2.042(2) . yes Fe1 C6 2.051(3) . yes Fe1 C1 2.055(2) . yes Fe1 C7 2.058(3) . yes Fe1 C10 2.066(3) . yes Fe1 C9 2.068(3) . yes Fe1 C8 2.068(3) . yes Fe1 C4 2.079(3) . yes Fe1 C3 2.079(3) . yes Fe2 C25 2.048(3) . yes Fe2 C22 2.051(2) . yes Fe2 C26 2.053(3) . yes Fe2 C28 2.055(3) . yes Fe2 C21 2.061(2) . yes Fe2 C29 2.064(3) . yes Fe2 C27 2.067(3) . yes Fe2 C30 2.070(3) . yes Fe2 C23 2.073(2) . yes Fe2 C24 2.076(3) . yes P F6 1.557(2) . ? P F4 1.569(2) . ? P F3 1.578(2) . ? P F5 1.579(2) . ? P F2 1.5988(19) . ? P F1 1.6006(18) . ? C1 C40 1.421(4) . ? C1 C5 1.450(4) . ? C1 C2 1.455(3) . ? C2 C3 1.418(4) . ? C2 C11 1.511(4) . ? C3 C4 1.437(4) . ? C3 C12 1.493(4) . ? C4 C5 1.412(3) . ? C4 C13 1.501(4) . ? C5 C14 1.499(4) . ? C6 C10 1.413(4) . ? C6 C7 1.420(4) . ? C6 H6 0.94(3) . ? C7 C8 1.434(4) . ? C7 C15 1.498(4) . ? C8 C9 1.431(4) . ? C8 C16 1.502(4) . ? C9 C10 1.429(4) . ? C9 C17 1.501(4) . ? C10 C18 1.495(4) . ? C11 H11A 0.97(3) . ? C11 H11B 0.98(3) . ? C11 H11C 0.99(3) . ? C12 H12A 1.00(4) . ? C12 H12B 1.05(3) . ? C12 H12C 0.86(3) . ? C13 H13A 0.96(3) . ? C13 H13B 1.01(3) . ? C13 H13C 0.96(3) . ? C14 H14A 0.90(3) . ? C14 H14B 0.99(3) . ? C14 H14C 1.00(3) . ? C15 H15A 0.96(3) . ? C15 H15B 1.07(3) . ? C15 H15C 0.97(3) . ? C16 H16A 0.92(3) . ? C16 H16B 0.97(3) . ? C16 H16C 1.08(3) . ? C17 H17A 0.95(4) . ? C17 H17B 0.98(3) . ? C17 H17C 0.99(3) . ? C18 H18A 0.92(3) . ? C18 H18B 0.95(3) . ? C18 H18C 0.97(3) . ? C21 C42 1.416(4) . ? C21 C25 1.448(3) . ? C21 C22 1.458(3) . ? C22 C23 1.421(4) . ? C22 C31 1.499(4) . ? C23 C24 1.430(4) . ? C23 C32 1.494(4) . ? C24 C25 1.419(4) . ? C24 C33 1.494(4) . ? C25 C34 1.495(4) . ? C26 C30 1.421(4) . ? C26 C27 1.429(4) . ? C26 H26 0.85(3) . ? C27 C28 1.420(4) . ? C27 C35 1.500(4) . ? C28 C29 1.443(4) . ? C28 C36 1.499(4) . ? C29 C30 1.421(4) . ? C29 C37 1.502(4) . ? C30 C38 1.494(4) . ? C31 H31A 0.99(3) . ? C31 H31B 0.94(3) . ? C31 H31C 1.04(3) . ? C32 H32A 0.91(3) . ? C32 H32B 1.02(3) . ? C32 H32C 0.95(3) . ? C33 H33A 0.93(3) . ? C33 H33B 0.94(3) . ? C33 H33C 1.02(3) . ? C34 H34A 0.93(3) . ? C34 H34B 1.00(3) . ? C34 H34C 0.90(3) . ? C35 H35A 1.05(3) . ? C35 H35C 0.96(4) . ? C35 H35B 0.93(3) . ? C36 H36A 0.91(4) . ? C36 H36B 1.00(4) . ? C36 H36C 1.17(4) . ? C37 H37A 1.02(4) . ? C37 H37B 1.01(3) . ? C37 H37C 0.88(4) . ? C38 H38A 0.88(3) . ? C38 H38B 0.94(3) . ? C38 H38C 1.12(4) . ? C40 C41 1.379(4) . ? C40 H40 0.92(3) . ? C41 C42 1.380(4) . ? C41 H41 0.87(2) . ? C42 H42 0.99(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 C2 Fe1 C5 69.97(10) . . ? C2 Fe1 C6 107.36(11) . . ? C5 Fe1 C6 173.60(11) . . ? C2 Fe1 C1 41.70(10) . . ? C5 Fe1 C1 41.45(10) . . ? C6 Fe1 C1 132.83(11) . . ? C2 Fe1 C7 127.11(10) . . ? C5 Fe1 C7 145.82(10) . . ? C6 Fe1 C7 40.43(11) . . ? C1 Fe1 C7 168.48(10) . . ? C2 Fe1 C10 117.77(11) . . ? C5 Fe1 C10 135.39(11) . . ? C6 Fe1 C10 40.15(11) . . ? C1 Fe1 C10 112.77(11) . . ? C7 Fe1 C10 68.05(11) . . ? C2 Fe1 C9 151.79(11) . . ? C5 Fe1 C9 111.58(10) . . ? C6 Fe1 C9 67.83(11) . . ? C1 Fe1 C9 120.28(10) . . ? C7 Fe1 C9 68.34(11) . . ? C10 Fe1 C9 40.45(11) . . ? C2 Fe1 C8 165.74(11) . . ? C5 Fe1 C8 116.14(10) . . ? C6 Fe1 C8 67.87(11) . . ? C1 Fe1 C8 150.82(10) . . ? C7 Fe1 C8 40.69(10) . . ? C10 Fe1 C8 67.94(11) . . ? C9 Fe1 C8 40.49(11) . . ? C2 Fe1 C4 68.45(10) . . ? C5 Fe1 C4 40.07(10) . . ? C6 Fe1 C4 145.10(11) . . ? C1 Fe1 C4 68.08(10) . . ? C7 Fe1 C4 112.82(10) . . ? C10 Fe1 C4 172.08(11) . . ? C9 Fe1 C4 131.90(11) . . ? C8 Fe1 C4 107.26(11) . . ? C2 Fe1 C3 40.34(10) . . ? C5 Fe1 C3 68.44(10) . . ? C6 Fe1 C3 113.58(11) . . ? C1 Fe1 C3 68.36(10) . . ? C7 Fe1 C3 104.47(10) . . ? C10 Fe1 C3 147.48(11) . . ? C9 Fe1 C3 167.84(11) . . ? C8 Fe1 C3 127.82(11) . . ? C4 Fe1 C3 40.44(10) . . ? C25 Fe2 C22 69.64(10) . . ? C25 Fe2 C26 140.95(11) . . ? C22 Fe2 C26 129.26(11) . . ? C25 Fe2 C28 113.46(11) . . ? C22 Fe2 C28 150.76(11) . . ? C26 Fe2 C28 68.01(11) . . ? C25 Fe2 C21 41.27(10) . . ? C22 Fe2 C21 41.55(10) . . ? C26 Fe2 C21 170.68(11) . . ? C28 Fe2 C21 120.77(11) . . ? C25 Fe2 C29 140.66(11) . . ? C22 Fe2 C29 117.41(11) . . ? C26 Fe2 C29 67.60(11) . . ? C28 Fe2 C29 41.01(11) . . ? C21 Fe2 C29 116.31(10) . . ? C25 Fe2 C27 113.80(10) . . ? C22 Fe2 C27 167.67(11) . . ? C26 Fe2 C27 40.60(11) . . ? C28 Fe2 C27 40.31(11) . . ? C21 Fe2 C27 148.11(10) . . ? C29 Fe2 C27 68.11(11) . . ? C25 Fe2 C30 177.82(11) . . ? C22 Fe2 C30 108.18(10) . . ? C26 Fe2 C30 40.33(10) . . ? C28 Fe2 C30 68.46(11) . . ? C21 Fe2 C30 137.06(10) . . ? C29 Fe2 C30 40.19(11) . . ? C27 Fe2 C30 68.30(10) . . ? C25 Fe2 C23 68.21(10) . . ? C22 Fe2 C23 40.32(10) . . ? C26 Fe2 C23 103.46(11) . . ? C28 Fe2 C23 168.87(10) . . ? C21 Fe2 C23 68.24(10) . . ? C29 Fe2 C23 143.83(11) . . ? C27 Fe2 C23 128.58(11) . . ? C30 Fe2 C23 110.11(11) . . ? C25 Fe2 C24 40.24(10) . . ? C22 Fe2 C24 68.44(10) . . ? C26 Fe2 C24 108.55(10) . . ? C28 Fe2 C24 133.89(11) . . ? C21 Fe2 C24 68.21(10) . . ? C29 Fe2 C24 174.11(11) . . ? C27 Fe2 C24 106.03(11) . . ? C30 Fe2 C24 139.23(11) . . ? C23 Fe2 C24 40.32(10) . . ? F6 P F4 91.25(18) . . ? F6 P F3 90.85(17) . . ? F4 P F3 177.90(19) . . ? F6 P F5 178.82(18) . . ? F4 P F5 89.93(17) . . ? F3 P F5 87.98(16) . . ? F6 P F2 90.57(12) . . ? F4 P F2 90.93(13) . . ? F3 P F2 89.23(13) . . ? F5 P F2 89.38(11) . . ? F6 P F1 90.21(12) . . ? F4 P F1 89.13(11) . . ? F3 P F1 90.68(12) . . ? F5 P F1 89.84(11) . . ? F2 P F1 179.21(11) . . ? C40 C1 C5 123.5(2) . . ? C40 C1 C2 128.6(2) . . ? C5 C1 C2 107.0(2) . . ? C40 C1 Fe1 119.77(18) . . ? C5 C1 Fe1 68.77(14) . . ? C2 C1 Fe1 68.31(13) . . ? C3 C2 C1 107.9(2) . . ? C3 C2 C11 124.1(2) . . ? C1 C2 C11 127.8(2) . . ? C3 C2 Fe1 71.60(14) . . ? C1 C2 Fe1 69.99(14) . . ? C11 C2 Fe1 127.77(19) . . ? C2 C3 C4 108.2(2) . . ? C2 C3 C12 126.5(2) . . ? C4 C3 C12 125.2(2) . . ? C2 C3 Fe1 68.06(14) . . ? C4 C3 Fe1 69.79(14) . . ? C12 C3 Fe1 129.35(19) . . ? C5 C4 C3 108.8(2) . . ? C5 C4 C13 126.3(2) . . ? C3 C4 C13 124.8(2) . . ? C5 C4 Fe1 68.53(14) . . ? C3 C4 Fe1 69.78(14) . . ? C13 C4 Fe1 129.21(19) . . ? C4 C5 C1 107.9(2) . . ? C4 C5 C14 126.3(2) . . ? C1 C5 C14 125.7(2) . . ? C4 C5 Fe1 71.40(14) . . ? C1 C5 Fe1 69.78(14) . . ? C14 C5 Fe1 127.47(19) . . ? C10 C6 C7 109.1(2) . . ? C10 C6 Fe1 70.50(15) . . ? C7 C6 Fe1 70.04(15) . . ? C10 C6 H6 126.0(17) . . ? C7 C6 H6 124.9(17) . . ? Fe1 C6 H6 126.5(16) . . ? C6 C7 C8 107.4(2) . . ? C6 C7 C15 126.8(3) . . ? C8 C7 C15 125.7(3) . . ? C6 C7 Fe1 69.53(15) . . ? C8 C7 Fe1 70.03(14) . . ? C15 C7 Fe1 129.1(2) . . ? C7 C8 C9 107.9(2) . . ? C7 C8 C16 126.0(3) . . ? C9 C8 C16 126.1(3) . . ? C7 C8 Fe1 69.29(15) . . ? C9 C8 Fe1 69.75(15) . . ? C16 C8 Fe1 128.5(2) . . ? C10 C9 C8 107.7(2) . . ? C10 C9 C17 126.6(3) . . ? C8 C9 C17 125.6(3) . . ? C10 C9 Fe1 69.73(15) . . ? C8 C9 Fe1 69.75(15) . . ? C17 C9 Fe1 128.2(2) . . ? C6 C10 C9 107.9(2) . . ? C6 C10 C18 125.7(3) . . ? C9 C10 C18 126.4(3) . . ? C6 C10 Fe1 69.34(15) . . ? C9 C10 Fe1 69.83(15) . . ? C18 C10 Fe1 127.7(2) . . ? C2 C11 H11A 106.1(18) . . ? C2 C11 H11B 114.4(16) . . ? H11A C11 H11B 108(2) . . ? C2 C11 H11C 109.9(17) . . ? H11A C11 H11C 108(2) . . ? H11B C11 H11C 110(2) . . ? C3 C12 H12A 108.9(19) . . ? C3 C12 H12B 107.8(17) . . ? H12A C12 H12B 109(2) . . ? C3 C12 H12C 112(2) . . ? H12A C12 H12C 111(3) . . ? H12B C12 H12C 108(3) . . ? C4 C13 H13A 110.6(16) . . ? C4 C13 H13B 113.0(17) . . ? H13A C13 H13B 112(2) . . ? C4 C13 H13C 115.1(18) . . ? H13A C13 H13C 102(2) . . ? H13B C13 H13C 104(2) . . ? C5 C14 H14A 110.0(18) . . ? C5 C14 H14B 115.2(18) . . ? H14A C14 H14B 105(3) . . ? C5 C14 H14C 109.5(16) . . ? H14A C14 H14C 105(2) . . ? H14B C14 H14C 112(2) . . ? C7 C15 H15A 110.7(19) . . ? C7 C15 H15B 112.6(18) . . ? H15A C15 H15B 107(2) . . ? C7 C15 H15C 111.9(18) . . ? H15A C15 H15C 108(3) . . ? H15B C15 H15C 106(3) . . ? C8 C16 H16A 112(2) . . ? C8 C16 H16B 109.2(19) . . ? H16A C16 H16B 101(3) . . ? C8 C16 H16C 109.6(16) . . ? H16A C16 H16C 113(3) . . ? H16B C16 H16C 112(2) . . ? C9 C17 H17A 113(2) . . ? C9 C17 H17B 113.4(18) . . ? H17A C17 H17B 107(3) . . ? C9 C17 H17C 113.8(18) . . ? H17A C17 H17C 102(3) . . ? H17B C17 H17C 107(3) . . ? C10 C18 H18A 111(2) . . ? C10 C18 H18B 109.2(18) . . ? H18A C18 H18B 107(3) . . ? C10 C18 H18C 106(2) . . ? H18A C18 H18C 110(3) . . ? H18B C18 H18C 114(3) . . ? C42 C21 C25 123.3(2) . . ? C42 C21 C22 128.8(2) . . ? C25 C21 C22 107.3(2) . . ? C42 C21 Fe2 120.20(18) . . ? C25 C21 Fe2 68.89(13) . . ? C22 C21 Fe2 68.85(14) . . ? C23 C22 C21 107.3(2) . . ? C23 C22 C31 124.4(2) . . ? C21 C22 C31 127.9(2) . . ? C23 C22 Fe2 70.68(14) . . ? C21 C22 Fe2 69.60(13) . . ? C31 C22 Fe2 130.49(19) . . ? C24 C23 C22 109.0(2) . . ? C24 C23 C32 125.2(2) . . ? C22 C23 C32 125.8(2) . . ? C24 C23 Fe2 69.96(14) . . ? C22 C23 Fe2 69.01(14) . . ? C32 C23 Fe2 128.14(19) . . ? C25 C24 C23 108.4(2) . . ? C25 C24 C33 125.9(2) . . ? C23 C24 C33 125.7(2) . . ? C25 C24 Fe2 68.83(15) . . ? C23 C24 Fe2 69.71(14) . . ? C33 C24 Fe2 127.06(18) . . ? C24 C25 C21 108.0(2) . . ? C24 C25 C34 126.5(2) . . ? C21 C25 C34 125.4(2) . . ? C24 C25 Fe2 70.93(14) . . ? C21 C25 Fe2 69.83(14) . . ? C34 C25 Fe2 127.47(19) . . ? C30 C26 C27 109.1(2) . . ? C30 C26 Fe2 70.50(15) . . ? C27 C26 Fe2 70.23(15) . . ? C30 C26 H26 123.6(19) . . ? C27 C26 H26 127.3(19) . . ? Fe2 C26 H26 125.8(19) . . ? C28 C27 C26 107.5(2) . . ? C28 C27 C35 126.8(3) . . ? C26 C27 C35 125.7(3) . . ? C28 C27 Fe2 69.41(15) . . ? C26 C27 Fe2 69.17(15) . . ? C35 C27 Fe2 128.1(2) . . ? C27 C28 C29 107.8(2) . . ? C27 C28 C36 125.9(3) . . ? C29 C28 C36 126.1(3) . . ? C27 C28 Fe2 70.28(15) . . ? C29 C28 Fe2 69.83(15) . . ? C36 C28 Fe2 128.8(2) . . ? C30 C29 C28 108.3(2) . . ? C30 C29 C37 125.7(3) . . ? C28 C29 C37 126.0(3) . . ? C30 C29 Fe2 70.13(15) . . ? C28 C29 Fe2 69.16(15) . . ? C37 C29 Fe2 127.8(2) . . ? C26 C30 C29 107.4(2) . . ? C26 C30 C38 125.1(3) . . ? C29 C30 C38 127.5(3) . . ? C26 C30 Fe2 69.16(15) . . ? C29 C30 Fe2 69.67(15) . . ? C38 C30 Fe2 125.8(2) . . ? C22 C31 H31A 111.2(16) . . ? C22 C31 H31B 107.0(18) . . ? H31A C31 H31B 103(2) . . ? C22 C31 H31C 112.3(15) . . ? H31A C31 H31C 107(2) . . ? H31B C31 H31C 116(2) . . ? C23 C32 H32A 112.2(18) . . ? C23 C32 H32B 110.1(17) . . ? H32A C32 H32B 110(3) . . ? C23 C32 H32C 113.7(18) . . ? H32A C32 H32C 102(2) . . ? H32B C32 H32C 108(2) . . ? C24 C33 H33A 111.9(18) . . ? C24 C33 H33B 110.4(18) . . ? H33A C33 H33B 114(3) . . ? C24 C33 H33C 118.5(19) . . ? H33A C33 H33C 104(2) . . ? H33B C33 H33C 98(2) . . ? C25 C34 H34A 113.7(17) . . ? C25 C34 H34B 111.6(17) . . ? H34A C34 H34B 104(2) . . ? C25 C34 H34C 111(2) . . ? H34A C34 H34C 106(2) . . ? H34B C34 H34C 110(3) . . ? C27 C35 H35A 108.2(19) . . ? C27 C35 H35C 108(2) . . ? H35A C35 H35C 114(3) . . ? C27 C35 H35B 114(2) . . ? H35A C35 H35B 101(2) . . ? H35C C35 H35B 112(3) . . ? C28 C36 H36A 107(2) . . ? C28 C36 H36B 114(2) . . ? H36A C36 H36B 104(3) . . ? C28 C36 H36C 114.6(17) . . ? H36A C36 H36C 113(3) . . ? H36B C36 H36C 105(3) . . ? C29 C37 H37A 114(2) . . ? C29 C37 H37B 107.2(17) . . ? H37A C37 H37B 113(3) . . ? C29 C37 H37C 109(2) . . ? H37A C37 H37C 100(3) . . ? H37B C37 H37C 113(3) . . ? C30 C38 H38A 109(2) . . ? C30 C38 H38B 115.1(18) . . ? H38A C38 H38B 98(3) . . ? C30 C38 H38C 113(2) . . ? H38A C38 H38C 112(3) . . ? H38B C38 H38C 110(3) . . ? C41 C40 C1 128.2(2) . . ? C41 C40 H40 114.6(17) . . ? C1 C40 H40 117.2(17) . . ? C40 C41 C42 121.7(2) . . ? C40 C41 H41 115.0(18) . . ? C42 C41 H41 123.1(18) . . ? C41 C42 C21 128.3(2) . . ? C41 C42 H42 114.7(15) . . ? C21 C42 H42 116.8(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.372 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.049 #===END data_3c _audit_creation_date 2001-08-29T13:31:19-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM _chemical_name_systematic ; 1,3-bis(ruthenocenyl)allylium tetrakis(3,5-bis(trifluoromethyl)phenyl)borate ; _chemical_name_common '3c, [Rc(CH)3Rc]+[BAr'4]-' _chemical_formula_moiety 'C55 H33 B1 F24 Ru2' _chemical_formula_sum 'C55 H33 B F24 Ru2' _chemical_formula_weight 1362.76 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.5037(6) _cell_length_b 18.7047(3) _cell_length_c 18.3623(5) _cell_angle_alpha 90 _cell_angle_beta 111.946(2) _cell_angle_gamma 90 _cell_volume 5257.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_special_details ; ? ; _exptl_absorpt_coefficient_mu 0.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8359 _exptl_absorpt_correction_T_max 0.8882 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 40156 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_unetI/netI 0.0706 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _reflns_number_total 11887 _reflns_number_gt 7206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+26.5058P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00025(13) _refine_ls_number_reflns 11887 _refine_ls_number_parameters 736 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1269 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1817 _refine_ls_wR_factor_gt 0.1437 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.24 _refine_diff_density_min -1.24 _refine_diff_density_rms 0.128 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 0 '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' F F 0.0171 0.0103 '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' 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 0.07253(3) 0.35250(3) 0.17430(3) 0.03312(15) Uani 1 1 d . . . Ru2 Ru 0.33890(3) 0.61629(3) 0.19991(3) 0.03779(16) Uani 1 1 d . . . C1 C -0.0423(7) 0.4190(6) 0.1374(7) 0.091(4) Uani 1 1 d . . . H1 H -0.0806 0.4222 0.1651 0.109 Uiso 1 1 calc R . . C2 C -0.0497(5) 0.3722(5) 0.0791(6) 0.070(3) Uani 1 1 d . . . H2 H -0.0924 0.3356 0.061 0.084 Uiso 1 1 calc R . . C3 C 0.0137(5) 0.3859(4) 0.0506(4) 0.0551(19) Uani 1 1 d . . . H3 H 0.0202 0.3616 0.0077 0.066 Uiso 1 1 calc R . . C4 C 0.0670(5) 0.4399(4) 0.0929(4) 0.0529(19) Uani 1 1 d . . . H4 H 0.117 0.4582 0.0852 0.064 Uiso 1 1 calc R . . C5 C 0.0342(8) 0.4635(4) 0.1504(5) 0.080(3) Uani 1 1 d . . . H5 H 0.057 0.5001 0.1885 0.096 Uiso 1 1 calc R . . C6 C 0.1484(6) 0.3273(4) 0.2945(4) 0.059(2) Uani 1 1 d . . . H6 H 0.1685 0.3623 0.3348 0.071 Uiso 1 1 calc R . . C7 C 0.0713(6) 0.2883(4) 0.2739(5) 0.060(2) Uani 1 1 d . . . H7 H 0.0289 0.2932 0.2971 0.072 Uiso 1 1 calc R . . C8 C 0.0663(5) 0.2411(4) 0.2137(5) 0.059(2) Uani 1 1 d . . . H8 H 0.0204 0.2079 0.1901 0.071 Uiso 1 1 calc R . . C9 C 0.1385(5) 0.2503(4) 0.1940(5) 0.056(2) Uani 1 1 d . . . H9 H 0.1508 0.2248 0.1546 0.068 Uiso 1 1 calc R . . C10 C 0.1918(5) 0.3051(4) 0.2437(5) 0.055(2) Uani 1 1 d . . . C11 C 0.2417(5) 0.3530(4) 0.2164(5) 0.056(2) Uani 1 1 d . . . H11 H 0.2482 0.3416 0.1685 0.067 Uiso 1 1 calc R . . C12 C 0.2833(4) 0.4179(4) 0.2566(4) 0.0463(17) Uani 1 1 d . . . H12 H 0.273 0.4354 0.3009 0.056 Uiso 1 1 calc R . . C13 C 0.3382(5) 0.4527(4) 0.2278(5) 0.0536(19) Uani 1 1 d . . . H13 H 0.346 0.4333 0.183 0.064 Uiso 1 1 calc R . . C14 C 0.3852(4) 0.5181(3) 0.2626(4) 0.0449(17) Uani 1 1 d . . . C15 C 0.4528(5) 0.5500(5) 0.2384(5) 0.059(2) Uani 1 1 d . . . H15 H 0.4762 0.5306 0.2025 0.071 Uiso 1 1 calc R . . C16 C 0.4759(4) 0.6159(4) 0.2795(4) 0.0446(16) Uani 1 1 d . . . H16 H 0.5184 0.6489 0.277 0.054 Uiso 1 1 calc R . . C17 C 0.4238(4) 0.6229(4) 0.3247(4) 0.0459(17) Uani 1 1 d . . . H17 H 0.4262 0.6624 0.3579 0.055 Uiso 1 1 calc R . . C18 C 0.3682(5) 0.5643(4) 0.3144(4) 0.0502(18) Uani 1 1 d . . . H18 H 0.3267 0.5573 0.3382 0.06 Uiso 1 1 calc R . . C19 C 0.2040(5) 0.6505(6) 0.1434(7) 0.084(3) Uani 1 1 d . . . H19 H 0.1603 0.6418 0.1643 0.1 Uiso 1 1 calc R . . C20 C 0.2254(6) 0.6065(5) 0.0921(6) 0.076(3) Uani 1 1 d . . . H20 H 0.1993 0.5616 0.0725 0.091 Uiso 1 1 calc R . . C21 C 0.2909(7) 0.6391(5) 0.0747(5) 0.072(3) Uani 1 1 d . . . H21 H 0.3168 0.6208 0.0402 0.086 Uiso 1 1 calc R . . C22 C 0.3131(5) 0.7040(4) 0.1162(5) 0.059(2) Uani 1 1 d . . . H22 H 0.3566 0.7369 0.1153 0.071 Uiso 1 1 calc R . . C23 C 0.2599(6) 0.7108(5) 0.1587(5) 0.068(2) Uani 1 1 d . . . H23 H 0.2605 0.7495 0.1924 0.081 Uiso 1 1 calc R . . B B 0.2362(4) 0.5156(3) 0.7235(4) 0.0214(12) Uani 1 1 d . . . C31 C 0.2527(3) 0.4459(3) 0.7818(3) 0.0197(10) Uani 1 1 d . . . C32 C 0.3135(3) 0.3922(3) 0.7876(3) 0.0212(11) Uani 1 1 d . . . H32 H 0.3454 0.3941 0.754 0.025 Uiso 1 1 calc R . . C33 C 0.3293(3) 0.3354(3) 0.8412(3) 0.0236(11) Uani 1 1 d . . . C34 C 0.2843(3) 0.3305(3) 0.8912(3) 0.0243(11) Uani 1 1 d . . . H34 H 0.294 0.2918 0.9271 0.029 Uiso 1 1 calc R . . C35 C 0.2248(4) 0.3839(3) 0.8870(3) 0.0257(11) Uani 1 1 d . . . C36 C 0.2099(3) 0.4402(3) 0.8345(3) 0.0249(11) Uani 1 1 d . . . H36 H 0.1692 0.4762 0.8343 0.03 Uiso 1 1 calc R . . C37 C 0.3971(4) 0.2819(3) 0.8436(3) 0.0293(13) Uani 1 1 d . . . F1 F 0.3895(2) 0.25995(18) 0.7711(2) 0.0397(8) Uani 1 1 d . . . F2 F 0.4786(2) 0.3068(2) 0.8771(2) 0.0461(9) Uani 1 1 d . . . F3 F 0.3928(2) 0.22285(19) 0.8831(2) 0.0458(10) Uani 1 1 d . . . C38 C 0.1771(5) 0.3814(4) 0.9423(4) 0.0443(17) Uani 1 1 d . . . F4 F 0.0907(4) 0.3766(5) 0.9030(4) 0.128(3) Uani 1 1 d . . . F5 F 0.1952(4) 0.3296(3) 0.9900(4) 0.113(3) Uani 1 1 d . . . F6 F 0.1788(6) 0.4404(3) 0.9776(5) 0.148(4) Uani 1 1 d . . . C41 C 0.1325(3) 0.5296(3) 0.6705(3) 0.0215(11) Uani 1 1 d . . . C42 C 0.0630(3) 0.4863(3) 0.6682(3) 0.0245(11) Uani 1 1 d . . . H42 H 0.0747 0.4448 0.7003 0.029 Uiso 1 1 calc R . . C43 C -0.0238(3) 0.5018(3) 0.6201(3) 0.0291(12) Uani 1 1 d . . . C44 C -0.0431(4) 0.5617(3) 0.5725(3) 0.0318(13) Uani 1 1 d . A . H44 H -0.1017 0.5724 0.5397 0.038 Uiso 1 1 calc R . . C45 C 0.0247(4) 0.6055(3) 0.5738(3) 0.0284(12) Uani 1 1 d . . . C46 C 0.1104(3) 0.5901(3) 0.6214(3) 0.0250(11) Uani 1 1 d . A . H46 H 0.1556 0.6214 0.621 0.03 Uiso 1 1 calc R . . C47 C -0.0972(4) 0.4551(3) 0.6209(4) 0.0413(16) Uani 1 1 d . . . F7 F -0.1418(4) 0.4272(4) 0.5532(4) 0.126(3) Uani 1 1 d . . . F8 F -0.1583(3) 0.4909(3) 0.6365(4) 0.097(2) Uani 1 1 d . . . F9 F -0.0749(3) 0.4060(4) 0.6727(5) 0.140(3) Uani 1 1 d . . . C48 C 0.0039(4) 0.6708(4) 0.5247(4) 0.0426(16) Uani 0.691(6) 1 d PD A 1 F10 F -0.0406(5) 0.7188(3) 0.5452(4) 0.0603(11) Uani 0.691(6) 1 d PD A 1 F11 F 0.0746(4) 0.7043(4) 0.5204(4) 0.0603(11) Uani 0.691(6) 1 d PD A 1 F12 F -0.0478(4) 0.6536(3) 0.4480(4) 0.0603(11) Uani 0.691(6) 1 d PD A 1 C48A C 0.0039(4) 0.6708(4) 0.5247(4) 0.0426(16) Uani 0.309(6) 1 d PD A 2 F10A F 0.0612(9) 0.6897(9) 0.4938(9) 0.0603(11) Uani 0.309(6) 1 d PD A 2 F11A F -0.0778(7) 0.6794(8) 0.4733(8) 0.0603(11) Uani 0.309(6) 1 d PD A 2 F12A F 0.0093(10) 0.7301(6) 0.5757(7) 0.0603(11) Uani 0.309(6) 1 d PD A 2 C51 C 0.2780(3) 0.5837(3) 0.7834(3) 0.0209(11) Uani 1 1 d . . . C52 C 0.3669(4) 0.5832(3) 0.8292(3) 0.0315(13) Uani 1 1 d . . . H52 H 0.4011 0.5441 0.824 0.038 Uiso 1 1 calc R . . C53 C 0.4079(4) 0.6374(3) 0.8823(4) 0.0381(15) Uani 1 1 d . . . C54 C 0.3599(4) 0.6940(3) 0.8940(4) 0.0340(14) Uani 1 1 d . . . H54 H 0.387 0.7306 0.9311 0.041 Uiso 1 1 calc R . . C55 C 0.2713(4) 0.6955(3) 0.8501(3) 0.0261(12) Uani 1 1 d . . . C56 C 0.2316(3) 0.6413(3) 0.7959(3) 0.0236(11) Uani 1 1 d . . . H56 H 0.1705 0.644 0.7665 0.028 Uiso 1 1 calc R . . C57 C 0.2171(4) 0.7564(3) 0.8606(4) 0.0356(14) Uani 1 1 d . . . F13 F 0.1430(3) 0.7645(3) 0.8005(4) 0.105(2) Uani 1 1 d . . . F14 F 0.1958(5) 0.7482(3) 0.9221(4) 0.105(2) Uani 1 1 d . . . F15 F 0.2567(3) 0.8186(2) 0.8701(3) 0.0696(14) Uani 1 1 d . . . C58 C 0.5046(5) 0.6342(5) 0.9273(6) 0.074(3) Uani 1 1 d . . . F16 F 0.5470(3) 0.6068(6) 0.8908(5) 0.209(6) Uani 1 1 d . . . F17 F 0.5227(4) 0.5884(3) 0.9914(5) 0.151(4) Uani 1 1 d . . . F18 F 0.5395(2) 0.6933(3) 0.9610(3) 0.0684(13) Uani 1 1 d . . . C61 C 0.2854(3) 0.5060(3) 0.6618(3) 0.0208(11) Uani 1 1 d . . . C62 C 0.3405(3) 0.5564(3) 0.6481(3) 0.0235(11) Uani 1 1 d . . . H62 H 0.3497 0.6006 0.6754 0.028 Uiso 1 1 calc R . . C63 C 0.3828(4) 0.5446(3) 0.5960(3) 0.0297(13) Uani 1 1 d . . . C64 C 0.3715(4) 0.4804(3) 0.5550(3) 0.0333(14) Uani 1 1 d . B . H64 H 0.4008 0.4714 0.5202 0.04 Uiso 1 1 calc R . . C65 C 0.3158(4) 0.4299(3) 0.5668(3) 0.0312(13) Uani 1 1 d . . . C66 C 0.2726(3) 0.4428(3) 0.6170(3) 0.0245(11) Uani 1 1 d . B . H66 H 0.2329 0.4079 0.6215 0.029 Uiso 1 1 calc R . . C67 C 0.4413(5) 0.6016(4) 0.5851(5) 0.0455(17) Uani 1 1 d . . . F19 F 0.4804(3) 0.6401(3) 0.6499(3) 0.0761(15) Uani 1 1 d . . . F20 F 0.5051(3) 0.5762(3) 0.5664(3) 0.0770(16) Uani 1 1 d . . . F21 F 0.3974(3) 0.6495(3) 0.5322(4) 0.0883(18) Uani 1 1 d . . . C68 C 0.3060(4) 0.3605(4) 0.5270(4) 0.0458(17) Uani 0.547(5) 1 d PD B 1 F22 F 0.2260(6) 0.3345(6) 0.5068(5) 0.0703(13) Uani 0.547(5) 1 d PD B 1 F23 F 0.3667(6) 0.3160(4) 0.5597(5) 0.0703(13) Uani 0.547(5) 1 d PD B 1 F24 F 0.3107(6) 0.3703(4) 0.4520(5) 0.0703(13) Uani 0.547(5) 1 d PD B 1 C68A C 0.3060(4) 0.3605(4) 0.5270(4) 0.0458(17) Uani 0.453(5) 1 d PD B 2 F22A F 0.3704(6) 0.3375(5) 0.5070(6) 0.0703(13) Uani 0.453(5) 1 d PD B 2 F23A F 0.2291(6) 0.3406(7) 0.4768(6) 0.0703(13) Uani 0.453(5) 1 d PD B 2 F24A F 0.3158(7) 0.3025(5) 0.5844(5) 0.0703(13) Uani 0.453(5) 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0337(3) 0.0319(3) 0.0355(3) 0.0000(2) 0.0150(2) 0.0024(2) Ru2 0.0293(3) 0.0393(3) 0.0426(3) 0.0100(2) 0.0109(2) 0.0013(2) C1 0.090(7) 0.097(8) 0.127(9) 0.076(7) 0.087(7) 0.070(6) C2 0.043(4) 0.076(6) 0.085(7) 0.037(5) 0.016(5) 0.010(4) C3 0.061(5) 0.062(5) 0.041(4) 0.007(4) 0.017(4) -0.003(4) C4 0.056(4) 0.058(5) 0.051(5) 0.014(4) 0.027(4) 0.002(4) C5 0.152(10) 0.035(4) 0.043(5) 0.011(3) 0.026(6) 0.037(5) C6 0.082(6) 0.049(4) 0.028(4) -0.004(3) 0.000(4) 0.005(4) C7 0.081(6) 0.051(5) 0.050(5) 0.016(4) 0.026(4) 0.002(4) C8 0.052(4) 0.029(4) 0.074(6) 0.009(4) -0.002(4) -0.007(3) C9 0.053(4) 0.044(4) 0.056(5) -0.012(3) 0.002(4) 0.017(4) C10 0.037(4) 0.046(4) 0.060(5) 0.013(4) -0.006(3) 0.001(3) C11 0.052(4) 0.053(4) 0.047(4) -0.007(4) 0.002(4) 0.014(4) C12 0.036(3) 0.040(4) 0.054(4) 0.005(3) 0.007(3) 0.006(3) C13 0.053(4) 0.052(4) 0.051(5) -0.005(4) 0.015(4) 0.019(4) C14 0.037(3) 0.033(4) 0.055(4) 0.012(3) 0.006(3) 0.002(3) C15 0.049(4) 0.071(5) 0.053(5) -0.003(4) 0.013(4) 0.029(4) C16 0.026(3) 0.050(4) 0.054(4) 0.006(3) 0.010(3) 0.001(3) C17 0.035(3) 0.062(5) 0.033(4) 0.007(3) 0.004(3) 0.002(3) C18 0.050(4) 0.052(4) 0.047(4) 0.005(3) 0.017(4) 0.006(4) C19 0.032(4) 0.118(9) 0.095(8) 0.062(7) 0.016(5) 0.024(5) C20 0.066(6) 0.060(6) 0.066(6) 0.018(5) -0.018(5) 0.000(5) C21 0.089(7) 0.077(6) 0.047(5) 0.016(4) 0.023(5) 0.027(6) C22 0.059(5) 0.052(5) 0.067(5) 0.032(4) 0.023(4) 0.007(4) C23 0.063(5) 0.062(5) 0.068(6) 0.021(4) 0.012(5) 0.027(5) B 0.019(3) 0.023(3) 0.023(3) -0.001(2) 0.009(2) -0.002(2) C31 0.018(2) 0.020(3) 0.019(3) -0.002(2) 0.005(2) -0.004(2) C32 0.021(2) 0.023(3) 0.020(3) 0.003(2) 0.009(2) 0.001(2) C33 0.020(2) 0.024(3) 0.027(3) 0.004(2) 0.010(2) 0.001(2) C34 0.027(3) 0.022(3) 0.022(3) 0.003(2) 0.008(2) 0.002(2) C35 0.030(3) 0.022(3) 0.032(3) 0.002(2) 0.020(2) 0.002(2) C36 0.025(3) 0.025(3) 0.027(3) 0.003(2) 0.012(2) 0.006(2) C37 0.030(3) 0.027(3) 0.035(3) 0.012(2) 0.018(3) 0.007(2) F1 0.048(2) 0.0366(19) 0.042(2) 0.0018(16) 0.0257(18) 0.0131(17) F2 0.0219(17) 0.052(2) 0.063(3) 0.0018(19) 0.0142(17) 0.0061(16) F3 0.056(2) 0.035(2) 0.062(3) 0.0241(18) 0.040(2) 0.0237(18) C38 0.056(4) 0.041(4) 0.052(4) 0.012(3) 0.040(4) 0.019(3) F4 0.069(4) 0.240(9) 0.106(5) 0.057(5) 0.068(4) 0.028(5) F5 0.164(6) 0.105(4) 0.137(5) 0.087(4) 0.133(5) 0.083(4) F6 0.302(11) 0.071(4) 0.186(7) -0.036(4) 0.223(8) -0.031(5) C41 0.022(2) 0.020(3) 0.023(3) -0.005(2) 0.009(2) -0.004(2) C42 0.026(3) 0.020(3) 0.024(3) 0.001(2) 0.005(2) 0.000(2) C43 0.023(3) 0.026(3) 0.035(3) 0.000(2) 0.007(2) -0.002(2) C44 0.022(3) 0.032(3) 0.033(3) 0.005(2) 0.001(2) 0.000(2) C45 0.030(3) 0.029(3) 0.023(3) 0.006(2) 0.005(2) 0.005(2) C46 0.026(3) 0.023(3) 0.026(3) 0.002(2) 0.009(2) -0.002(2) C47 0.026(3) 0.032(3) 0.057(4) 0.003(3) 0.005(3) -0.005(3) F7 0.126(5) 0.171(7) 0.105(5) -0.084(5) 0.070(4) -0.120(5) F8 0.068(3) 0.076(4) 0.179(6) -0.019(4) 0.084(4) -0.017(3) F9 0.038(3) 0.119(5) 0.223(8) 0.119(5) 0.004(4) -0.021(3) C48 0.031(3) 0.049(4) 0.042(4) 0.012(3) 0.007(3) 0.005(3) F10 0.068(2) 0.048(2) 0.058(3) 0.0252(18) 0.015(2) 0.0107(17) F11 0.068(2) 0.048(2) 0.058(3) 0.0252(18) 0.015(2) 0.0107(17) F12 0.068(2) 0.048(2) 0.058(3) 0.0252(18) 0.015(2) 0.0107(17) C48A 0.031(3) 0.049(4) 0.042(4) 0.012(3) 0.007(3) 0.005(3) F10A 0.068(2) 0.048(2) 0.058(3) 0.0252(18) 0.015(2) 0.0107(17) F11A 0.068(2) 0.048(2) 0.058(3) 0.0252(18) 0.015(2) 0.0107(17) F12A 0.068(2) 0.048(2) 0.058(3) 0.0252(18) 0.015(2) 0.0107(17) C51 0.026(3) 0.021(3) 0.017(3) 0.002(2) 0.011(2) -0.001(2) C52 0.028(3) 0.030(3) 0.035(3) -0.009(3) 0.009(3) 0.004(2) C53 0.027(3) 0.044(4) 0.037(4) -0.012(3) 0.004(3) -0.003(3) C54 0.029(3) 0.038(3) 0.034(3) -0.016(3) 0.011(3) -0.006(3) C55 0.032(3) 0.020(3) 0.027(3) -0.005(2) 0.012(2) -0.004(2) C56 0.023(2) 0.022(3) 0.027(3) -0.001(2) 0.011(2) -0.004(2) C57 0.035(3) 0.028(3) 0.048(4) -0.011(3) 0.020(3) -0.006(3) F13 0.065(3) 0.080(4) 0.125(5) -0.059(3) -0.018(3) 0.042(3) F14 0.165(6) 0.066(3) 0.152(6) 0.022(3) 0.137(5) 0.045(4) F15 0.061(3) 0.030(2) 0.132(4) -0.023(2) 0.053(3) -0.004(2) C58 0.034(4) 0.085(7) 0.082(7) -0.050(6) -0.005(4) 0.006(4) F16 0.020(2) 0.380(14) 0.198(8) -0.226(9) 0.007(4) 0.003(4) F17 0.084(4) 0.073(4) 0.190(8) 0.008(5) -0.069(5) 0.008(3) F18 0.031(2) 0.076(3) 0.076(3) -0.026(3) -0.006(2) -0.015(2) C61 0.022(2) 0.019(2) 0.020(3) 0.002(2) 0.006(2) 0.005(2) C62 0.027(3) 0.020(3) 0.024(3) 0.000(2) 0.010(2) -0.001(2) C63 0.031(3) 0.032(3) 0.033(3) 0.011(2) 0.018(3) 0.006(2) C64 0.036(3) 0.044(4) 0.024(3) 0.003(3) 0.016(3) 0.013(3) C65 0.029(3) 0.032(3) 0.028(3) -0.008(2) 0.005(2) 0.006(3) C66 0.026(3) 0.022(3) 0.023(3) -0.004(2) 0.006(2) -0.005(2) C67 0.049(4) 0.041(4) 0.060(5) 0.011(3) 0.038(4) 0.005(3) F19 0.082(3) 0.077(3) 0.088(4) -0.021(3) 0.054(3) -0.050(3) F20 0.073(3) 0.061(3) 0.136(5) -0.001(3) 0.084(3) -0.005(2) F21 0.072(3) 0.079(3) 0.111(4) 0.063(3) 0.031(3) 0.004(3) C68 0.033(3) 0.054(4) 0.041(4) -0.023(3) 0.004(3) 0.011(3) F22 0.088(3) 0.058(2) 0.063(3) -0.039(2) 0.026(2) -0.001(2) F23 0.088(3) 0.058(2) 0.063(3) -0.039(2) 0.026(2) -0.001(2) F24 0.088(3) 0.058(2) 0.063(3) -0.039(2) 0.026(2) -0.001(2) C68A 0.033(3) 0.054(4) 0.041(4) -0.023(3) 0.004(3) 0.011(3) F22A 0.088(3) 0.058(2) 0.063(3) -0.039(2) 0.026(2) -0.001(2) F23A 0.088(3) 0.058(2) 0.063(3) -0.039(2) 0.026(2) -0.001(2) F24A 0.088(3) 0.058(2) 0.063(3) -0.039(2) 0.026(2) -0.001(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 C10 2.100(7) . ? Ru1 C6 2.143(7) . ? Ru1 C2 2.150(8) . ? Ru1 C1 2.153(8) . ? Ru1 C9 2.163(7) . ? Ru1 C5 2.167(7) . ? Ru1 C4 2.193(7) . ? Ru1 C7 2.193(7) . ? Ru1 C3 2.200(7) . ? Ru1 C8 2.221(7) . ? Ru1 C11 2.604(8) . ? Ru2 C15 2.139(7) . ? Ru2 C14 2.151(6) . ? Ru2 C23 2.159(8) . ? Ru2 C20 2.166(8) . ? Ru2 C19 2.171(7) . ? Ru2 C21 2.176(8) . ? Ru2 C22 2.178(7) . ? Ru2 C16 2.185(6) . ? Ru2 C17 2.197(7) . ? Ru2 C18 2.199(7) . ? Ru2 C13 3.104(8) . ? C1 C2 1.352(15) . ? C1 C5 1.456(15) . ? C2 C3 1.357(12) . ? C3 C4 1.374(11) . ? C4 C5 1.425(12) . ? C6 C7 1.390(12) . ? C6 C10 1.433(12) . ? C7 C8 1.392(12) . ? C8 C9 1.380(12) . ? C9 C10 1.435(10) . ? C10 C11 1.428(11) . ? C11 C12 1.452(10) . ? C12 C13 1.372(10) . ? C13 C14 1.462(10) . ? C14 C18 1.388(10) . ? C14 C15 1.474(11) . ? C15 C16 1.420(11) . ? C16 C17 1.405(10) . ? C17 C18 1.397(10) . ? C19 C20 1.392(15) . ? C19 C23 1.416(13) . ? C20 C21 1.380(14) . ? C21 C22 1.407(13) . ? C22 C23 1.382(12) . ? B C61 1.633(8) . ? B C41 1.643(7) . ? B C31 1.644(8) . ? B C51 1.655(8) . ? C31 C32 1.396(7) . ? C31 C36 1.399(7) . ? C32 C33 1.405(7) . ? C33 C34 1.383(7) . ? C33 C37 1.489(7) . ? C34 C35 1.383(7) . ? C35 C36 1.387(8) . ? C35 C38 1.500(8) . ? C37 F2 1.337(7) . ? C37 F3 1.338(6) . ? C37 F1 1.353(7) . ? C38 F5 1.264(8) . ? C38 F6 1.276(9) . ? C38 F4 1.339(10) . ? C41 C42 1.392(7) . ? C41 C46 1.407(7) . ? C42 C43 1.403(7) . ? C43 C44 1.382(8) . ? C43 C47 1.499(8) . ? C44 C45 1.380(8) . ? C45 C46 1.387(8) . ? C45 C48 1.480(8) . ? C47 F9 1.273(8) . ? C47 F7 1.295(8) . ? C47 F8 1.327(8) . ? C48 F10 1.301(8) . ? C48 F11 1.353(8) . ? C48 F12 1.384(8) . ? C51 C56 1.389(7) . ? C51 C52 1.392(8) . ? C52 C53 1.395(8) . ? C53 C54 1.386(9) . ? C53 C58 1.500(9) . ? C54 C55 1.381(8) . ? C55 C56 1.400(7) . ? C55 C57 1.505(8) . ? C57 F14 1.311(8) . ? C57 F15 1.314(7) . ? C57 F13 1.315(8) . ? C58 F16 1.246(10) . ? C58 F18 1.294(9) . ? C58 F17 1.394(13) . ? C61 C62 1.395(7) . ? C61 C66 1.411(7) . ? C62 C63 1.395(8) . ? C63 C64 1.393(8) . ? C63 C67 1.502(9) . ? C64 C65 1.390(9) . ? C65 C66 1.381(8) . ? C65 C68 1.469(8) . ? C67 F20 1.313(7) . ? C67 F21 1.320(8) . ? C67 F19 1.334(9) . ? C68 F23 1.270(9) . ? C68 F22 1.323(9) . ? C68 F24 1.419(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Ru1 C6 39.5(3) . . ? C10 Ru1 C2 161.3(4) . . ? C6 Ru1 C2 152.1(4) . . ? C10 Ru1 C1 161.8(5) . . ? C6 Ru1 C1 123.9(4) . . ? C2 Ru1 C1 36.6(4) . . ? C10 Ru1 C9 39.3(3) . . ? C6 Ru1 C9 64.5(3) . . ? C2 Ru1 C9 123.2(4) . . ? C1 Ru1 C9 153.1(4) . . ? C10 Ru1 C5 131.6(4) . . ? C6 Ru1 C5 115.7(3) . . ? C2 Ru1 C5 63.7(4) . . ? C1 Ru1 C5 39.4(4) . . ? C9 Ru1 C5 166.3(4) . . ? C10 Ru1 C4 121.2(3) . . ? C6 Ru1 C4 136.4(3) . . ? C2 Ru1 C4 62.0(3) . . ? C1 Ru1 C4 63.1(3) . . ? C9 Ru1 C4 131.5(3) . . ? C5 Ru1 C4 38.2(3) . . ? C10 Ru1 C7 64.0(3) . . ? C6 Ru1 C7 37.4(3) . . ? C2 Ru1 C7 118.2(3) . . ? C1 Ru1 C7 107.3(3) . . ? C9 Ru1 C7 62.5(3) . . ? C5 Ru1 C7 126.9(3) . . ? C4 Ru1 C7 164.7(3) . . ? C10 Ru1 C3 134.3(3) . . ? C6 Ru1 C3 171.0(3) . . ? C2 Ru1 C3 36.3(3) . . ? C1 Ru1 C3 60.9(4) . . ? C9 Ru1 C3 115.1(3) . . ? C5 Ru1 C3 62.4(3) . . ? C4 Ru1 C3 36.4(3) . . ? C7 Ru1 C3 151.3(3) . . ? C10 Ru1 C8 63.5(3) . . ? C6 Ru1 C8 62.5(3) . . ? C2 Ru1 C8 106.4(3) . . ? C1 Ru1 C8 120.1(4) . . ? C9 Ru1 C8 36.7(3) . . ? C5 Ru1 C8 156.8(4) . . ? C4 Ru1 C8 157.8(3) . . ? C7 Ru1 C8 36.8(3) . . ? C3 Ru1 C8 123.1(3) . . ? C10 Ru1 C11 33.2(3) . . ? C6 Ru1 C11 63.0(3) . . ? C2 Ru1 C11 144.8(3) . . ? C1 Ru1 C11 144.2(4) . . ? C9 Ru1 C11 62.4(3) . . ? C5 Ru1 C11 104.8(4) . . ? C4 Ru1 C11 88.1(3) . . ? C7 Ru1 C11 95.6(3) . . ? C3 Ru1 C11 108.4(3) . . ? C8 Ru1 C11 94.7(3) . . ? C15 Ru2 C14 40.2(3) . . ? C15 Ru2 C23 158.6(4) . . ? C14 Ru2 C23 159.1(3) . . ? C15 Ru2 C20 127.3(4) . . ? C14 Ru2 C20 115.4(3) . . ? C23 Ru2 C20 63.0(4) . . ? C15 Ru2 C19 161.1(4) . . ? C14 Ru2 C19 127.1(3) . . ? C23 Ru2 C19 38.2(4) . . ? C20 Ru2 C19 37.4(4) . . ? C15 Ru2 C21 113.0(3) . . ? C14 Ru2 C21 130.5(3) . . ? C23 Ru2 C21 62.3(4) . . ? C20 Ru2 C21 37.1(4) . . ? C19 Ru2 C21 62.2(4) . . ? C15 Ru2 C22 125.8(3) . . ? C14 Ru2 C22 163.2(3) . . ? C23 Ru2 C22 37.1(3) . . ? C20 Ru2 C22 62.9(3) . . ? C19 Ru2 C22 63.0(3) . . ? C21 Ru2 C22 37.7(3) . . ? C15 Ru2 C16 38.3(3) . . ? C14 Ru2 C16 64.4(3) . . ? C23 Ru2 C16 125.2(3) . . ? C20 Ru2 C16 159.4(4) . . ? C19 Ru2 C16 160.0(4) . . ? C21 Ru2 C16 125.8(3) . . ? C22 Ru2 C16 110.8(3) . . ? C15 Ru2 C17 63.2(3) . . ? C14 Ru2 C17 61.9(3) . . ? C23 Ru2 C17 112.7(3) . . ? C20 Ru2 C17 162.7(4) . . ? C19 Ru2 C17 128.5(4) . . ? C21 Ru2 C17 158.3(3) . . ? C22 Ru2 C17 125.0(3) . . ? C16 Ru2 C17 37.4(3) . . ? C15 Ru2 C18 64.9(3) . . ? C14 Ru2 C18 37.2(3) . . ? C23 Ru2 C18 125.9(3) . . ? C20 Ru2 C18 129.9(4) . . ? C19 Ru2 C18 114.0(3) . . ? C21 Ru2 C18 163.7(3) . . ? C22 Ru2 C18 157.3(3) . . ? C16 Ru2 C18 63.6(3) . . ? C17 Ru2 C18 37.1(3) . . ? C15 Ru2 C13 55.4(3) . . ? C14 Ru2 C13 24.8(2) . . ? C23 Ru2 C13 145.7(3) . . ? C20 Ru2 C13 90.7(3) . . ? C19 Ru2 C13 107.7(3) . . ? C21 Ru2 C13 110.2(3) . . ? C22 Ru2 C13 147.9(3) . . ? C16 Ru2 C13 87.3(2) . . ? C17 Ru2 C13 85.7(2) . . ? C18 Ru2 C13 54.5(2) . . ? C2 C1 C5 108.4(7) . . ? C2 C1 Ru1 71.6(5) . . ? C5 C1 Ru1 70.8(5) . . ? C1 C2 C3 109.2(9) . . ? C1 C2 Ru1 71.8(6) . . ? C3 C2 Ru1 73.8(5) . . ? C2 C3 C4 110.1(8) . . ? C2 C3 Ru1 69.8(5) . . ? C4 C3 Ru1 71.5(4) . . ? C3 C4 C5 107.8(8) . . ? C3 C4 Ru1 72.1(4) . . ? C5 C4 Ru1 69.9(4) . . ? C4 C5 C1 104.3(8) . . ? C4 C5 Ru1 71.9(4) . . ? C1 C5 Ru1 69.8(4) . . ? C7 C6 C10 107.5(7) . . ? C7 C6 Ru1 73.3(4) . . ? C10 C6 Ru1 68.6(4) . . ? C6 C7 C8 109.0(8) . . ? C6 C7 Ru1 69.3(4) . . ? C8 C7 Ru1 72.7(4) . . ? C9 C8 C7 109.2(7) . . ? C9 C8 Ru1 69.4(4) . . ? C7 C8 Ru1 70.6(4) . . ? C8 C9 C10 107.8(7) . . ? C8 C9 Ru1 73.9(4) . . ? C10 C9 Ru1 68.0(4) . . ? C11 C10 C6 122.7(7) . . ? C11 C10 C9 121.5(8) . . ? C6 C10 C9 106.5(7) . . ? C11 C10 Ru1 93.2(4) . . ? C6 C10 Ru1 71.9(4) . . ? C9 C10 Ru1 72.7(4) . . ? C10 C11 C12 124.8(8) . . ? C10 C11 Ru1 53.6(4) . . ? C12 C11 Ru1 113.9(5) . . ? C13 C12 C11 117.1(7) . . ? C12 C13 C14 123.1(7) . . ? C12 C13 Ru2 125.1(5) . . ? C14 C13 Ru2 38.1(3) . . ? C18 C14 C13 127.7(7) . . ? C18 C14 C15 108.9(6) . . ? C13 C14 C15 123.0(7) . . ? C18 C14 Ru2 73.3(4) . . ? C13 C14 Ru2 117.1(5) . . ? C15 C14 Ru2 69.5(4) . . ? C16 C15 C14 105.9(6) . . ? C16 C15 Ru2 72.6(4) . . ? C14 C15 Ru2 70.4(4) . . ? C17 C16 C15 107.1(7) . . ? C17 C16 Ru2 71.8(4) . . ? C15 C16 Ru2 69.1(4) . . ? C18 C17 C16 111.2(7) . . ? C18 C17 Ru2 71.6(4) . . ? C16 C17 Ru2 70.8(4) . . ? C14 C18 C17 106.9(7) . . ? C14 C18 Ru2 69.5(4) . . ? C17 C18 Ru2 71.4(4) . . ? C20 C19 C23 107.2(8) . . ? C20 C19 Ru2 71.1(5) . . ? C23 C19 Ru2 70.5(4) . . ? C21 C20 C19 108.3(9) . . ? C21 C20 Ru2 71.9(5) . . ? C19 C20 Ru2 71.5(5) . . ? C20 C21 C22 108.9(9) . . ? C20 C21 Ru2 71.1(5) . . ? C22 C21 Ru2 71.2(5) . . ? C23 C22 C21 107.1(8) . . ? C23 C22 Ru2 70.7(4) . . ? C21 C22 Ru2 71.1(4) . . ? C22 C23 C19 108.6(9) . . ? C22 C23 Ru2 72.2(5) . . ? C19 C23 Ru2 71.4(5) . . ? C61 B C41 106.5(4) . . ? C61 B C31 111.1(4) . . ? C41 B C31 113.3(4) . . ? C61 B C51 110.7(4) . . ? C41 B C51 110.8(4) . . ? C31 B C51 104.5(4) . . ? C32 C31 C36 115.3(5) . . ? C32 C31 B 124.0(4) . . ? C36 C31 B 120.5(4) . . ? C31 C32 C33 122.5(5) . . ? C34 C33 C32 120.7(5) . . ? C34 C33 C37 121.3(5) . . ? C32 C33 C37 118.0(5) . . ? C33 C34 C35 117.5(5) . . ? C34 C35 C36 121.7(5) . . ? C34 C35 C38 118.8(5) . . ? C36 C35 C38 119.5(5) . . ? C35 C36 C31 122.3(5) . . ? F2 C37 F3 106.6(5) . . ? F2 C37 F1 105.4(4) . . ? F3 C37 F1 106.2(5) . . ? F2 C37 C33 113.3(5) . . ? F3 C37 C33 112.3(4) . . ? F1 C37 C33 112.5(5) . . ? F5 C38 F6 110.9(7) . . ? F5 C38 F4 104.5(7) . . ? F6 C38 F4 98.5(7) . . ? F5 C38 C35 116.4(5) . . ? F6 C38 C35 113.6(6) . . ? F4 C38 C35 111.1(6) . . ? C42 C41 C46 115.8(5) . . ? C42 C41 B 126.1(5) . . ? C46 C41 B 118.1(4) . . ? C41 C42 C43 122.3(5) . . ? C44 C43 C42 120.4(5) . . ? C44 C43 C47 118.8(5) . . ? C42 C43 C47 120.8(5) . . ? C45 C44 C43 118.4(5) . . ? C44 C45 C46 121.2(5) . . ? C44 C45 C48 118.5(5) . . ? C46 C45 C48 120.3(5) . . ? C45 C46 C41 122.0(5) . . ? F9 C47 F7 109.2(7) . . ? F9 C47 F8 103.6(7) . . ? F7 C47 F8 101.9(6) . . ? F9 C47 C43 114.8(5) . . ? F7 C47 C43 113.4(6) . . ? F8 C47 C43 112.9(5) . . ? F10 C48 F11 106.9(6) . . ? F10 C48 F12 104.7(5) . . ? F11 C48 F12 105.4(6) . . ? F10 C48 C45 114.9(6) . . ? F11 C48 C45 114.1(5) . . ? F12 C48 C45 110.0(5) . . ? C56 C51 C52 115.4(5) . . ? C56 C51 B 126.0(5) . . ? C52 C51 B 118.6(5) . . ? C51 C52 C53 122.9(5) . . ? C54 C53 C52 120.5(5) . . ? C54 C53 C58 119.9(6) . . ? C52 C53 C58 119.6(6) . . ? C55 C54 C53 117.8(5) . . ? C54 C55 C56 120.9(5) . . ? C54 C55 C57 119.3(5) . . ? C56 C55 C57 119.8(5) . . ? C51 C56 C55 122.5(5) . . ? F14 C57 F15 105.8(6) . . ? F14 C57 F13 105.7(6) . . ? F15 C57 F13 105.7(6) . . ? F14 C57 C55 112.6(5) . . ? F15 C57 C55 113.4(5) . . ? F13 C57 C55 113.0(5) . . ? F16 C58 F18 111.7(9) . . ? F16 C58 F17 102.5(10) . . ? F18 C58 F17 101.8(7) . . ? F16 C58 C53 114.7(7) . . ? F18 C58 C53 114.8(7) . . ? F17 C58 C53 109.7(8) . . ? C62 C61 C66 115.2(5) . . ? C62 C61 B 125.3(5) . . ? C66 C61 B 119.5(5) . . ? C63 C62 C61 122.9(5) . . ? C64 C63 C62 120.4(5) . . ? C64 C63 C67 120.2(5) . . ? C62 C63 C67 119.4(5) . . ? C65 C64 C63 117.7(5) . . ? C66 C65 C64 121.4(5) . . ? C66 C65 C68 119.9(6) . . ? C64 C65 C68 118.7(5) . . ? C65 C66 C61 122.2(5) . . ? F20 C67 F21 109.1(6) . . ? F20 C67 F19 105.2(6) . . ? F21 C67 F19 103.9(6) . . ? F20 C67 C63 113.3(6) . . ? F21 C67 C63 112.1(6) . . ? F19 C67 C63 112.6(6) . . ? F23 C68 F22 114.8(8) . . ? F23 C68 F24 102.9(6) . . ? F22 C68 F24 100.7(6) . . ? F23 C68 C65 115.1(6) . . ? F22 C68 C65 112.2(6) . . ? F24 C68 C65 109.5(6) . . ? #===END data_4a _audit_creation_method CRYM _chemical_name_systematic ; 1-ferrocenyl-3-(2,3,4,5,1',2',3'4'-octamethylferrocenyl)allylium tetrafluoroborate ; _chemical_name_common '4a, [Fc(CH)3Fc"]+[BF4]-' _chemical_formula_moiety 'C31 H37 B1 F4 Fe2' _chemical_formula_structural 'C31 H37 B1 F4 Fe2' _chemical_formula_sum 'C31 H37 B1 F4 Fe2' _chemical_formula_weight 608.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source 'C' 'C' 'International Tables Vol C Table 4.2.6.8 and Vol IV Table 2.2B' 'H' 'H' 'International Tables Vol C Table 4.2.6.8 and Vol IV Table 2.2B' 'B' 'B' 'International Tables Vol C Table 4.2.6.8 and Vol IV Table 2.2B' 'F' 'F' 'International Tables Vol C Table 4.2.6.8 and Vol IV Table 2.2B' 'Fe' 'Fe' 'International Tables Vol C Table 4.2.6.8 and Vol IV Table 2.2B' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '1/2-x,1/2+y,1/2-z' '1/2+x,1/2-y,1/2+z' _cell_length_a 8.702(3) _cell_length_b 20.419(4) _cell_length_c 15.446(3) _cell_angle_alpha 90 _cell_angle_beta 93.24(2) _cell_angle_gamma 90 _cell_volume 2740.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 85 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.3 _cell_measurement_theta_max 14.2 _exptl_crystal_description Fragment _exptl_crystal_colour 'Green' _exptl_crystal_size_min ? _exptl_crystal_size_mid ? _exptl_crystal_size_max ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'Not measured' _exptl_crystal_F_000 ? _exptl_absorpt_coefficient_mu 1.104 _exptl_absorpt_correction_type '\Y-scan (North, Phillips & Matthews, 1968)' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 1.05 _exptl_special_details ; ? ; _diffrn_ambient_temperature 85 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_source 'Normal focus sealed tube' _diffrn_radiation_monochromator Graphite _diffrn_measurement_device_type CAD-4 _diffrn_measurement_method '\W scans' _diffrn_standards_number 3 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.8 _diffrn_reflns_number 11091 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.0 _diffrn_reflns_theta_max 25.0 _reflns_number_total 4830 _reflns_number_observed 4830 _reflns_observed_criterion All _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'CRYM (Duchamp, 1964)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'CRYM (Duchamp, 1964)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'CRYM (Duchamp, 1964)' _refine_special_details ; Weights w are calculated as 1/\s^2(Fo^2); variances (\s^2(Fo^2)) were derived from counting statistics plus an additional term, (0.014I)^2; variances of the merged data were obtained by propagation of error plus another additional term, (0.014)^2. 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. Duchamp, D. J. (1964). Am. Crystallogr. Assoc. Meet., Bozeman, Montana., Paper B14, 29-30. Enraf-Nonius. (1989). CAD-4 Software. Version 5. Enraf-Nonius, Delft, The Netherlands. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. North, A. C. T., Phillips, D. C., Matthews, F. S. (1968). Acta. Cryst., A24, 351-359. Sheldrick, G. M. (1990). Acta Crystallogr., A46, 467-473. ; _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^) _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method None _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_number_reflns 4830 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_obs 0.0594 _refine_ls_wR_factor_all 0.1132 _refine_ls_wR_factor_obs 0.1132 _refine_ls_goodness_of_fit_all 2.73 _refine_ls_goodness_of_fit_obs 2.73 _refine_ls_shift/esd_max 0.00 _refine_ls_shift/esd_mean ? _refine_diff_density_max 1.21 _refine_diff_density_min -0.80 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.23620(7) 0.99356(3) 0.87791(4) 0.02260(10) Uani 1 d . . Fe2 Fe 0.12386(6) 0.81677(2) 0.48244(3) 0.01490(10) Uani 1 d . . C1 C 0.1198(5) 0.9347(2) 0.9590(3) 0.0311(10) Uani 1 d . . C2 C 0.2595(6) 0.9559(2) 1.0007(3) 0.0317(11) Uani 1 d . . C3 C 0.3817(5) 0.9339(2) 0.9508(3) 0.0286(10) Uani 1 d . . C4 C 0.3166(5) 0.8996(2) 0.8780(3) 0.0264(10) Uani 1 d . . C5 C 0.1552(5) 0.9001(2) 0.8834(3) 0.0292(11) Uani 1 d . . C6 C 0.1635(6) 1.0327(2) 0.7630(3) 0.0325(12) Uani 1 d . . C7 C 0.0930(6) 1.0651(2) 0.8347(3) 0.0399(12) Uani 1 d . . C8 C 0.2129(7) 1.0930(2) 0.8857(3) 0.0410(15) Uani 1 d . . C9 C 0.3522(6) 1.0782(2) 0.8506(3) 0.0429(13) Uani 1 d . . C10 C 0.3250(6) 1.0413(2) 0.7760(3) 0.0384(11) Uani 1 d . . C11 C 0.1122(5) 0.7172(2) 0.4746(3) 0.0230(10) Uani 1 d . . C12 C 0.0364(4) 0.7381(2) 0.5487(3) 0.0195(8) Uani 1 d . . C13 C 0.1476(5) 0.7712(2) 0.6037(2) 0.0211(9) Uani 1 d . . C14 C 0.2899(5) 0.7711(2) 0.5627(3) 0.0254(9) Uani 1 d . . C15 C 0.2684(5) 0.7375(2) 0.4831(3) 0.0275(10) Uani 1 d . . C16 C 0.0613(5) 0.9125(2) 0.4809(3) 0.0248(11) Uani 1 d . . C17 C -0.0558(5) 0.8728(2) 0.4359(3) 0.0274(10) Uani 1 d . . C18 C 0.0135(6) 0.8427(2) 0.3655(3) 0.0320(12) Uani 1 d . . C19 C 0.1687(5) 0.8647(2) 0.3668(3) 0.0334(11) Uani 1 d . . C20 C 0.1992(5) 0.9055(2) 0.4379(3) 0.0313(11) Uani 1 d . . C21 C 0.0788(5) 0.9926(2) 0.6988(3) 0.0341(10) Uani 1 d . . C22 C 0.1379(5) 0.9672(2) 0.6249(3) 0.0213(9) Uani 1 d . . C23 C 0.0372(5) 0.9336(2) 0.5662(3) 0.0299(11) Uani 1 d . . C24 C -0.2234(5) 0.8675(2) 0.4536(3) 0.0389(12) Uani 1 d . . C25 C -0.0634(7) 0.7968(2) 0.3009(3) 0.0534(15) Uani 1 d . . C26 C 0.2801(7) 0.8493(3) 0.2976(3) 0.0561(15) Uani 1 d . . C27 C 0.3512(5) 0.9406(2) 0.4596(3) 0.0425(13) Uani 1 d . . C28 C -0.1279(5) 0.7244(2) 0.5672(3) 0.0282(10) Uani 1 d . . C29 C 0.1185(6) 0.7992(2) 0.6912(3) 0.0336(11) Uani 1 d . . C30 C 0.4407(5) 0.7990(2) 0.5988(3) 0.0441(13) Uani 1 d . . C31 C 0.3920(6) 0.7218(2) 0.4225(3) 0.0443(12) Uani 1 d . . B B 0.1804(7) 0.5850(3) 0.2436(4) 0.049(2) Uani 1 d . . F1 F 0.1204(5) 0.6343(2) 0.2888(2) 0.0980(12) Uani 1 d . . F2 F 0.0596(6) 0.5624(2) 0.1897(3) 0.0987(13) Uani 1 d . . F3 F 0.2310(5) 0.5354(3) 0.2912(4) 0.1517(19) Uani 1 d . . F4 F 0.2862(5) 0.6110(2) 0.1936(3) 0.1185(14) Uani 1 d . . H1 H 0.020 0.942 0.978 0.036 Uiso 1 calc . . H2 H 0.270 0.980 1.053 0.036 Uiso 1 calc . . H3 H 0.488 0.941 0.964 0.033 Uiso 1 calc . . H4 H 0.372 0.880 0.833 0.030 Uiso 1 calc . . H5 H 0.083 0.881 0.843 0.034 Uiso 1 calc . . H7 H -0.014 1.067 0.845 0.046 Uiso 1 calc . . H8 H 0.201 1.118 0.937 0.047 Uiso 1 calc . . H9 H 0.451 1.091 0.874 0.049 Uiso 1 calc . . H10 H 0.401 1.025 0.740 0.044 Uiso 1 calc . . H11 H 0.066 0.693 0.427 0.026 Uiso 1 calc . . H21 H -0.026 0.983 0.709 0.039 Uiso 1 calc . . H22 H 0.244 0.972 0.614 0.024 Uiso 1 calc . . H23 H -0.061 0.924 0.587 0.034 Uiso 1 calc . . H24a H -0.233 0.872 0.514 0.044 Uiso 1 calc . . H24b H -0.259 0.826 0.435 0.044 Uiso 1 calc . . H24c H -0.277 0.901 0.423 0.044 Uiso 1 calc . . H25a H 0.012 0.767 0.282 0.061 Uiso 1 calc . . H25b H -0.105 0.822 0.254 0.061 Uiso 1 calc . . H25c H -0.142 0.774 0.329 0.061 Uiso 1 calc . . H26a H 0.379 0.844 0.325 0.063 Uiso 1 calc . . H26b H 0.279 0.885 0.258 0.063 Uiso 1 calc . . H26c H 0.247 0.810 0.269 0.063 Uiso 1 calc . . H27a H 0.425 0.925 0.422 0.048 Uiso 1 calc . . H27b H 0.382 0.932 0.518 0.048 Uiso 1 calc . . H27c H 0.336 0.986 0.451 0.048 Uiso 1 calc . . H28a H -0.130 0.688 0.604 0.032 Uiso 1 calc . . H28b H -0.184 0.715 0.514 0.032 Uiso 1 calc . . H28c H -0.169 0.762 0.594 0.032 Uiso 1 calc . . H29a H 0.191 0.833 0.704 0.038 Uiso 1 calc . . H29b H 0.130 0.765 0.733 0.038 Uiso 1 calc . . H29c H 0.017 0.816 0.689 0.038 Uiso 1 calc . . H30a H 0.494 0.816 0.552 0.049 Uiso 1 calc . . H30b H 0.498 0.765 0.627 0.049 Uiso 1 calc . . H30c H 0.419 0.832 0.639 0.049 Uiso 1 calc . . H31a H 0.451 0.687 0.447 0.049 Uiso 1 calc . . H31b H 0.454 0.760 0.417 0.049 Uiso 1 calc . . H31c H 0.345 0.710 0.368 0.049 Uiso 1 calc . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.0308(3) 0.0176(3) 0.0191(3) -0.0021(3) -0.0012(3) -0.0021(2) Fe2 0.0162(3) 0.0136(3) 0.0149(3) 0.0014(2) 0.0008(2) 0.0012(2) C1 0.040(3) 0.028(2) 0.027(2) -0.005(2) 0.011(2) 0.000(2) C2 0.048(3) 0.026(2) 0.021(2) -0.003(2) 0.002(2) 0.001(2) C3 0.035(3) 0.024(2) 0.026(2) 0.002(2) -0.002(2) 0.004(2) C4 0.038(3) 0.016(2) 0.025(2) 0.002(2) 0.005(2) 0.001(2) C5 0.045(3) 0.019(2) 0.024(2) -0.011(2) 0.004(2) -0.003(2) C6 0.058(3) 0.018(2) 0.020(2) -0.003(2) -0.019(2) 0.001(2) C7 0.039(3) 0.032(3) 0.048(3) 0.011(2) -0.002(3) 0.011(2) C8 0.073(4) 0.017(2) 0.032(3) 0.005(2) -0.014(3) -0.007(2) C9 0.059(4) 0.026(2) 0.042(3) -0.015(2) -0.013(3) 0.010(2) C10 0.045(3) 0.033(3) 0.038(3) -0.005(2) 0.004(2) 0.016(2) C11 0.036(3) 0.013(2) 0.021(2) 0.001(2) 0.004(2) 0.002(2) C12 0.023(2) 0.015(2) 0.020(2) 0.002(2) 0.004(2) 0.005(2) C13 0.026(2) 0.017(2) 0.020(2) 0.002(2) 0.000(2) 0.009(2) C14 0.021(2) 0.024(2) 0.030(2) 0.001(2) -0.004(2) 0.014(2) C15 0.029(2) 0.020(2) 0.034(3) 0.013(2) 0.013(2) 0.013(2) C16 0.038(3) 0.011(2) 0.024(2) 0.002(2) -0.006(2) 0.000(2) C17 0.017(2) 0.026(2) 0.039(3) 0.006(2) 0.000(2) 0.017(2) C18 0.056(3) 0.019(2) 0.018(2) 0.002(2) -0.020(2) 0.001(2) C19 0.041(3) 0.038(3) 0.023(2) 0.017(2) 0.014(2) 0.016(2) C20 0.025(2) 0.022(2) 0.046(3) -0.001(2) -0.007(2) 0.016(2) C21 0.038(3) 0.030(2) 0.034(3) 0.003(2) -0.005(2) 0.008(2) C22 0.023(2) 0.017(2) 0.023(2) -0.002(2) -0.004(2) 0.001(2) C23 0.029(2) 0.021(2) 0.040(3) 0.002(2) -0.004(2) 0.007(2) C24 0.027(3) 0.034(3) 0.054(3) 0.001(2) -0.009(2) 0.004(2) C25 0.081(4) 0.041(3) 0.035(3) -0.001(3) -0.021(3) -0.002(2) C26 0.069(4) 0.062(4) 0.038(3) 0.011(3) 0.018(3) 0.015(3) C27 0.026(3) 0.040(3) 0.061(3) -0.002(2) 0.006(2) 0.010(3) C28 0.027(2) 0.024(2) 0.034(3) -0.001(2) 0.006(2) 0.007(2) C29 0.048(3) 0.032(2) 0.020(2) -0.001(2) -0.002(2) 0.004(2) C30 0.027(3) 0.054(3) 0.050(3) -0.004(2) -0.010(2) 0.028(3) C31 0.043(3) 0.035(3) 0.057(3) 0.021(2) 0.027(3) 0.013(2) B 0.043(4) 0.060(4) 0.047(4) 0.009(3) 0.024(3) 0.002(3) F1 0.102(3) 0.113(3) 0.083(3) -0.011(3) 0.037(3) -0.056(2) F2 0.153(4) 0.066(2) 0.075(3) -0.026(3) -0.017(3) 0.001(2) F3 0.090(3) 0.191(5) 0.176(5) 0.036(3) 0.027(3) 0.138(4) F4 0.102(3) 0.102(3) 0.162(4) 0.015(3) 0.099(3) 0.034(3) _geom_special_details ; ? ; 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 Fe1 Cp1 1.652 . . Fe1 Cp2 1.643 . . Fe2 Cp*1 1.675 . . Fe2 Cp*2 1.666 . . Fe1 C1 2.046(4) . . Fe1 C2 2.046(4) . . Fe1 C3 2.048(4) . . Fe1 C4 2.042(4) . . Fe1 C5 2.038(4) . . Fe1 C6 2.016(4) . . Fe1 C7 2.010(5) . . Fe1 C8 2.044(5) . . Fe1 C9 2.057(5) . . Fe1 C10 2.040(5) . . Fe2 C11 2.039(4) . . Fe2 C12 2.073(4) . . Fe2 C13 2.092(4) . . Fe2 C14 2.072(4) . . Fe2 C15 2.049(4) . . Fe2 C16 2.028(4) . . Fe2 C17 2.036(4) . . Fe2 C18 2.066(4) . . Fe2 C19 2.093(4) . . Fe2 C20 2.059(4) . . Fe1 C21 3.017(4) . . Fe2 C23 2.837(4) . . C1 C2 1.412(6) . . C1 C5 1.414(6) . . C1 H1 0.95 . . C2 C3 1.421(6) . . C2 H2 0.95 . . C3 C4 1.416(6) . . C3 H3 0.95 . . C4 C5 1.411(6) . . C4 H4 0.95 . . C5 H5 0.95 . . C6 C7 1.456(6) . . C6 C10 1.419(6) . . C6 C21 1.453(6) . . C7 C8 1.392(7) . . C7 H7 0.95 . . C8 C9 1.389(7) . . C8 H8 0.95 . . C9 C10 1.386(7) . . C9 H9 0.95 . . C10 H10 0.95 . . C11 C12 1.419(5) . . C11 C15 1.421(6) . . C11 H11 0.95 . . C12 C13 1.422(5) . . C12 C28 1.499(6) . . C13 C14 1.423(5) . . C13 C29 1.502(6) . . C14 C15 1.411(6) . . C14 C30 1.508(6) . . C15 C31 1.500(6) . . C16 C17 1.448(6) . . C16 C20 1.411(6) . . C16 C23 1.414(6) . . C17 C18 1.413(6) . . C17 C24 1.502(6) . . C18 C19 1.422(6) . . C18 C25 1.500(7) . . C19 C20 1.392(6) . . C19 C26 1.516(7) . . C20 C27 1.525(6) . . C21 C22 1.380(6) . . C21 H21 0.95 . . C22 C23 1.403(6) . . C22 H22 0.95 . . C23 H23 0.95 . . C24 H24a 0.95 . . C24 H24b 0.95 . . C24 H24c 0.95 . . C25 H25a 0.95 . . C25 H25b 0.95 . . C25 H25c 0.95 . . C26 H26a 0.94 . . C26 H26b 0.95 . . C26 H26c 0.95 . . C27 H27a 0.95 . . C27 H27b 0.95 . . C27 H27c 0.95 . . C28 H28a 0.95 . . C28 H28b 0.95 . . C28 H28c 0.95 . . C29 H29a 0.95 . . C29 H29b 0.95 . . C29 H29c 0.95 . . C30 H30a 0.95 . . C30 H30b 0.95 . . C30 H30c 0.95 . . C31 H31a 0.95 . . C31 H31b 0.95 . . C31 H31c 0.95 . . B F1 1.348(8) . . B F2 1.382(8) . . B F3 1.312(8) . . B F4 1.344(8) . . 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 C1 C2 107.9(4) . . . H1 C1 C2 126.1 . . . H1 C1 C5 126.1 . . . C3 C2 C1 107.9(4) . . . H2 C2 C1 126.1 . . . H2 C2 C3 126.1 . . . C4 C3 C2 108.0(4) . . . H3 C3 C2 126.0 . . . H3 C3 C4 126.0 . . . C5 C4 C3 107.7(4) . . . H4 C4 C3 126.1 . . . H4 C4 C5 126.1 . . . C4 C5 C1 108.5(4) . . . H5 C5 C1 125.8 . . . H5 C5 C4 125.8 . . . C10 C6 C7 107.0(4) . . . C21 C6 C7 123.8(4) . . . C21 C6 C10 128.8(4) . . . C8 C7 C6 106.4(4) . . . H7 C7 C6 126.8 . . . H7 C7 C8 126.8 . . . C9 C8 C7 109.5(4) . . . H8 C8 C7 125.3 . . . H8 C8 C9 125.3 . . . C10 C9 C8 109.3(4) . . . H9 C9 C8 125.3 . . . H9 C9 C10 125.3 . . . C9 C10 C6 107.8(4) . . . H10 C10 C6 126.1 . . . H10 C10 C9 126.1 . . . C15 C11 C12 108.9(3) . . . H11 C11 C12 125.6 . . . H11 C11 C15 125.6 . . . C13 C12 C11 107.1(3) . . . C28 C12 C11 126.1(3) . . . C28 C12 C13 126.8(3) . . . C14 C13 C12 108.2(3) . . . C29 C13 C12 125.1(3) . . . C29 C13 C14 126.7(4) . . . C15 C14 C13 108.3(3) . . . C30 C14 C13 126.5(4) . . . C30 C14 C15 125.1(4) . . . C14 C15 C11 107.5(3) . . . C31 C15 C11 126.6(4) . . . C31 C15 C14 125.7(4) . . . C20 C16 C17 108.2(4) . . . C23 C16 C17 118.8(4) . . . C23 C16 C20 130.1(4) . . . C18 C17 C16 107.0(4) . . . C24 C17 C16 128.1(4) . . . C24 C17 C18 124.7(4) . . . C19 C18 C17 107.4(4) . . . C25 C18 C17 126.1(4) . . . C25 C18 C19 126.5(4) . . . C20 C19 C18 109.8(4) . . . C26 C19 C18 124.7(4) . . . C26 C19 C20 125.4(4) . . . C19 C20 C16 107.6(4) . . . C27 C20 C16 126.8(4) . . . C27 C20 C19 125.4(4) . . . C22 C21 C6 125.3(4) . . . H21 C21 C6 117.4 . . . H21 C21 C22 117.4 . . . C23 C22 C21 118.0(4) . . . H22 C22 C21 121.0 . . . H22 C22 C23 121.0 . . . C22 C23 C16 129.2(4) . . . H23 C23 C16 115.4 . . . H23 C23 C22 115.4 . . . H24a C24 C17 108.4 . . . H24b C24 C17 108.4 . . . H24c C24 C17 108.4 . . . H24b C24 H24a 110.4 . . . H24c C24 H24a 110.6 . . . H24c C24 H24b 110.7 . . . H25a C25 C18 108.2 . . . H25b C25 C18 108.1 . . . H25c C25 C18 108.2 . . . H25b C25 H25a 110.8 . . . H25c C25 H25a 110.8 . . . H25c C25 H25b 110.7 . . . H26a C26 C19 108.4 . . . H26b C26 C19 108.2 . . . H26c C26 C19 108.2 . . . H26b C26 H26a 110.9 . . . H26c C26 H26a 110.8 . . . H26c C26 H26b 110.3 . . . H27a C27 C20 108.3 . . . H27b C27 C20 108.5 . . . H27c C27 C20 108.4 . . . H27b C27 H27a 110.5 . . . H27c C27 H27a 110.3 . . . H27c C27 H27b 110.7 . . . H28a C28 C12 108.4 . . . H28b C28 C12 108.4 . . . H28c C28 C12 108.4 . . . H28b C28 H28a 110.4 . . . H28c C28 H28a 110.6 . . . H28c C28 H28b 110.5 . . . H29a C29 C13 108.4 . . . H29b C29 C13 108.4 . . . H29c C29 C13 108.4 . . . H29b C29 H29a 110.5 . . . H29c C29 H29a 110.4 . . . H29c C29 H29b 110.5 . . . H30a C30 C14 108.2 . . . H30b C30 C14 108.2 . . . H30c C30 C14 108.3 . . . H30b C30 H30a 110.5 . . . H30c C30 H30a 110.8 . . . H30c C30 H30b 110.6 . . . H31a C31 C15 108.3 . . . H31b C31 C15 108.3 . . . H31c C31 C15 108.5 . . . H31b C31 H31a 110.4 . . . H31c C31 H31a 110.7 . . . H31c C31 H31b 110.6 . . . F2 B F1 104.9(5) . . . F3 B F1 114.4(6) . . . F4 B F1 107.4(5) . . . F3 B F2 107.5(5) . . . F4 B F2 108.0(5) . . . F4 B F3 114.1(6) . . . #===END data_5b _audit_creation_method SHELXL-97 _chemical_name_systematic ; '1-(ruthenocenyl)-3-(ferrocenyl)allylium hexafluorophosphate' ; _chemical_name_common '5b, [Rc(CH)3Fc]+[PF6]-' _chemical_formula_moiety 'C23 H21 F6 Fe P Ru' _chemical_formula_sum 'C23 H21 F6 Fe P Ru' _chemical_formula_weight 599.29 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.411(6) _cell_length_b 14.753(3) _cell_length_c 11.900(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.92(2) _cell_angle_gamma 90.00 _cell_volume 4270.7(17) _cell_formula_units_Z 8 _cell_measurement_temperature 84 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17 _cell_measurement_theta_max 19 _exptl_crystal_description Plate _exptl_crystal_colour 'Dark brown' _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.864 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 1.522 _exptl_absorpt_correction_type '\Y-scan (North, Phillips & Matthews, 1968)' _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 1.08 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 84 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD-4 _diffrn_measurement_method \W-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 75 _diffrn_standards_decay_% 'Within counting statistics' _diffrn_reflns_number 10102 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 25 _reflns_number_total 3753 _reflns_number_gt 3322 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'CRYM (Duchamp, 1964)' _computing_structure_solution none _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP/PC (Siemens, 1989)' _computing_publication_material ? _refine_special_details ; Data were collected with 1 degree \w-scans. The individual backgrounds were replaced by a background function of two theta derived from those reflections with I < 3\s(I). The GOF_merge was 1.20 (3753 multiples); R_int was 0.0172 for 2957 duplicates. Two outlier reflections (4 0 0, -9 3 3) were deleted from the dataset. The hexafluorophosphate anion occupies two different Wyckoff sites of multiplicity 4. Both sites are disordered. The PF6 at site e (0 y 1/4, point symmetry 2) is split 0.51(5):0.49(5) and the PF6 at site c (1/4, 1/4, 0, center of inversion) is split 0.88(2):0.12(2). The two fluorines with lowest site population (F2A, F3A) were refined isotropically. The bisruthenocenyl allyl hexafluorophosphate and 1-ferrocenyl 3-ruthenocenyl compounds are isostructural. The primary differences are the shorter Fe-C bonds (the single Cp ring on the ferrocenyl is displaced towards the allyl Cp ring approximately 0.3 Angstroms) and the slightly different disorder ratios of the PF6 on the center. The largest positive peak (1.21) in the final difference map is 0.83 Angstroms from the Fe atom. Weights w are calculated as 1/\s^2(Fo^2); variances (\s^2(Fo^2)) were derived from counting statistics plus an additional term, (0.014I)^2; variances of the merged data were obtained by propagation of error plus another additional term, (0.014)^2. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Isostructural with Ru-Ru analogue' _atom_sites_solution_secondary none _atom_sites_solution_hydrogens 'Isostructural with Ru-Ru analogue' _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3753 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 2.322 _refine_ls_restrained_S_all 2.322 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.144426(12) 0.090743(19) 0.19695(3) 0.01272(10) Uani 1 1 d . . . Fe Fe 0.40473(2) 0.10362(3) 0.40506(5) 0.01172(13) Uani 1 1 d . . . C1 C 0.14433(18) -0.0592(2) 0.1996(4) 0.0200(9) Uani 1 1 d . . . C2 C 0.11552(17) -0.0263(3) 0.0786(4) 0.0205(9) Uani 1 1 d . . . C3 C 0.15372(17) 0.0241(3) 0.0442(4) 0.0203(9) Uani 1 1 d . . . C4 C 0.20532(16) 0.0241(3) 0.1445(4) 0.0200(9) Uani 1 1 d . . . C5 C 0.19888(17) -0.0275(3) 0.2394(4) 0.0197(9) Uani 1 1 d . . . C6 C 0.10113(16) 0.1544(3) 0.2977(4) 0.0191(9) Uani 1 1 d . . . C7 C 0.06771(16) 0.1645(3) 0.1726(4) 0.0198(9) Uani 1 1 d . . . C8 C 0.09675(17) 0.2138(3) 0.1148(4) 0.0206(9) Uani 1 1 d . . . C9 C 0.14915(17) 0.2371(2) 0.2016(4) 0.0191(8) Uani 1 1 d . . . C10 C 0.15365(15) 0.1975(2) 0.3175(3) 0.0161(8) Uani 1 1 d . . . C11 C 0.20220(16) 0.1510(3) 0.3905(3) 0.0172(8) Uani 1 1 d . . . C12 C 0.25653(16) 0.1753(3) 0.3990(3) 0.0168(8) Uani 1 1 d . . . C13 C 0.30278(16) 0.1352(3) 0.4755(3) 0.0171(8) Uani 1 1 d . . . C14 C 0.35784(15) 0.1617(2) 0.4900(3) 0.0145(8) Uani 1 1 d . . . C15 C 0.37242(16) 0.2268(2) 0.4174(4) 0.0171(8) Uani 1 1 d . . . C16 C 0.43037(16) 0.2330(3) 0.4633(4) 0.0188(8) Uani 1 1 d . . . C17 C 0.45243(16) 0.1714(2) 0.5627(4) 0.0177(8) Uani 1 1 d . . . C18 C 0.40841(16) 0.1269(2) 0.5791(4) 0.0171(8) Uani 1 1 d . . . C19 C 0.36197(17) -0.0038(3) 0.3007(4) 0.0242(9) Uani 1 1 d . . . C20 C 0.36709(17) 0.0677(3) 0.2246(4) 0.0249(9) Uani 1 1 d . . . C21 C 0.42367(17) 0.0837(3) 0.2556(4) 0.0231(9) Uani 1 1 d . . . C22 C 0.45411(17) 0.0222(3) 0.3504(4) 0.0206(9) Uani 1 1 d . . . C23 C 0.41650(17) -0.0312(3) 0.3779(4) 0.0227(9) Uani 1 1 d . . . P1 P 0.2500 0.2500 0.0000 0.0197(3) Uani 1 2 d S . . F1 F 0.26280(10) 0.23695(18) 0.1420(2) 0.0327(6) Uani 1 1 d . A . F2 F 0.31443(16) 0.2614(5) 0.0325(3) 0.0325(14) Uani 0.881(18) 1 d P A 1 F3 F 0.2557(3) 0.1424(2) -0.0104(3) 0.0347(16) Uani 0.881(18) 1 d P A 1 F2A F 0.3051(11) 0.299(2) 0.039(2) 0.018(7) Uiso 0.119(18) 1 d P A 2 F3A F 0.2787(16) 0.158(2) -0.027(3) 0.039(9) Uiso 0.119(18) 1 d P A 2 P2 P 0.5000 0.39821(9) 0.2500 0.0159(3) Uani 1 2 d S . . F4 F 0.50671(10) 0.39861(16) 0.1219(2) 0.0299(6) Uani 1 1 d . B . F5 F 0.4436(7) 0.343(2) 0.1952(12) 0.051(5) Uani 0.51(5) 1 d P B 3 F6 F 0.4648(13) 0.4891(11) 0.2067(12) 0.052(5) Uani 0.51(5) 1 d P . 3 F5A F 0.4674(15) 0.3072(13) 0.2066(10) 0.057(6) Uani 0.49(5) 1 d P . 4 F6A F 0.4467(6) 0.453(2) 0.1938(15) 0.054(6) Uani 0.49(5) 1 d P B 4 H1 H 0.124(2) -0.099(4) 0.241(5) 0.064 Uiso 1 1 d . . . H2 H 0.081(2) -0.032(4) 0.042(5) 0.064 Uiso 1 1 d . . . H3 H 0.143(2) 0.052(4) -0.034(5) 0.064 Uiso 1 1 d . . . H4 H 0.237(2) 0.049(4) 0.155(5) 0.064 Uiso 1 1 d . . . H5 H 0.224(2) -0.034(4) 0.309(5) 0.064 Uiso 1 1 d . . . H6 H 0.093(2) 0.117(4) 0.356(5) 0.064 Uiso 1 1 d . . . H7 H 0.033(2) 0.142(4) 0.133(5) 0.064 Uiso 1 1 d . . . H8 H 0.082(2) 0.226(4) 0.033(5) 0.064 Uiso 1 1 d . . . H9 H 0.182(2) 0.269(4) 0.187(5) 0.064 Uiso 1 1 d . . . H11 H 0.200(2) 0.107(4) 0.454(5) 0.064 Uiso 1 1 d . . . H12 H 0.260(2) 0.227(4) 0.340(5) 0.064 Uiso 1 1 d . . . H13 H 0.300(2) 0.088(4) 0.533(5) 0.064 Uiso 1 1 d . . . H15 H 0.349(2) 0.264(4) 0.346(5) 0.064 Uiso 1 1 d . . . H16 H 0.448(2) 0.270(4) 0.423(5) 0.064 Uiso 1 1 d . . . H17 H 0.490(2) 0.157(4) 0.602(5) 0.064 Uiso 1 1 d . . . H18 H 0.409(2) 0.085(4) 0.640(5) 0.064 Uiso 1 1 d . . . H19 H 0.327(2) -0.024(4) 0.298(5) 0.064 Uiso 1 1 d . . . H20 H 0.338(2) 0.104(4) 0.161(5) 0.064 Uiso 1 1 d . . . H21 H 0.439(2) 0.131(4) 0.219(5) 0.064 Uiso 1 1 d . . . H22 H 0.492(2) 0.019(4) 0.392(5) 0.064 Uiso 1 1 d . . . H23 H 0.426(2) -0.070(4) 0.441(5) 0.064 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.01825(17) 0.00937(15) 0.01170(16) -0.00077(12) 0.00709(12) -0.00035(12) Fe 0.0152(3) 0.0073(3) 0.0116(3) -0.0028(2) 0.0041(2) 0.0015(2) C1 0.035(2) 0.0083(17) 0.021(2) -0.0029(16) 0.0152(19) 0.0004(17) C2 0.026(2) 0.015(2) 0.021(2) -0.0094(17) 0.0096(18) -0.0038(17) C3 0.036(2) 0.016(2) 0.016(2) -0.0022(16) 0.0169(19) 0.0018(17) C4 0.021(2) 0.015(2) 0.029(2) -0.0040(17) 0.0153(19) 0.0030(16) C5 0.028(2) 0.0102(18) 0.020(2) -0.0042(16) 0.0088(18) 0.0046(17) C6 0.022(2) 0.017(2) 0.021(2) -0.0044(17) 0.0106(18) 0.0028(17) C7 0.018(2) 0.0155(19) 0.023(2) -0.0023(16) 0.0049(18) 0.0040(16) C8 0.026(2) 0.0137(19) 0.021(2) 0.0029(17) 0.0077(18) 0.0074(17) C9 0.028(2) 0.0079(17) 0.022(2) -0.0022(16) 0.0112(18) 0.0024(16) C10 0.021(2) 0.0121(18) 0.0161(19) -0.0092(15) 0.0078(16) 0.0004(15) C11 0.024(2) 0.0139(19) 0.0141(19) -0.0071(16) 0.0075(17) -0.0033(16) C12 0.023(2) 0.0135(18) 0.015(2) -0.0067(16) 0.0082(17) -0.0011(16) C13 0.026(2) 0.0140(19) 0.0133(19) -0.0051(16) 0.0092(17) -0.0009(16) C14 0.019(2) 0.0112(18) 0.0129(19) -0.0039(15) 0.0059(16) -0.0012(15) C15 0.026(2) 0.0116(18) 0.0147(19) 0.0003(15) 0.0092(17) 0.0029(16) C16 0.025(2) 0.0145(19) 0.019(2) -0.0014(16) 0.0103(17) 0.0007(16) C17 0.020(2) 0.0132(18) 0.017(2) -0.0050(16) 0.0045(17) 0.0014(16) C18 0.024(2) 0.0097(18) 0.017(2) -0.0008(15) 0.0077(17) 0.0017(16) C19 0.024(2) 0.019(2) 0.027(2) -0.0124(18) 0.0072(19) -0.0001(18) C20 0.030(2) 0.022(2) 0.019(2) -0.0075(17) 0.0048(19) 0.0053(18) C21 0.033(2) 0.021(2) 0.018(2) -0.0033(17) 0.0125(18) 0.0049(18) C22 0.020(2) 0.019(2) 0.019(2) -0.0061(17) 0.0030(17) 0.0026(17) C23 0.032(2) 0.0128(19) 0.022(2) -0.0059(17) 0.0098(19) 0.0029(17) P1 0.0249(8) 0.0237(8) 0.0100(7) 0.0036(6) 0.0063(6) -0.0060(6) F1 0.0357(14) 0.0502(16) 0.0120(12) 0.0084(11) 0.0090(11) -0.0057(12) F2 0.0252(18) 0.052(3) 0.0202(17) 0.0074(17) 0.0088(13) -0.0032(19) F3 0.051(3) 0.0238(17) 0.0209(17) 0.0034(13) 0.0043(16) -0.0006(16) P2 0.0171(7) 0.0151(7) 0.0157(7) 0.000 0.0069(6) 0.000 F4 0.0337(13) 0.0416(15) 0.0184(12) -0.0017(11) 0.0143(11) 0.0083(12) F5 0.045(6) 0.077(11) 0.035(4) -0.030(5) 0.019(4) -0.035(7) F6 0.101(12) 0.033(6) 0.036(4) 0.014(4) 0.040(6) 0.045(6) F5A 0.099(14) 0.034(6) 0.039(4) -0.010(4) 0.027(6) -0.050(7) F6A 0.041(6) 0.089(15) 0.041(5) 0.039(7) 0.029(5) 0.040(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C10 2.080(3) . ? Ru C3 2.162(4) . ? Ru C9 2.162(4) . ? Ru C6 2.167(4) . ? Ru C2 2.171(4) . ? Ru C4 2.174(4) . ? Ru C5 2.191(4) . ? Ru C8 2.208(4) . ? Ru C1 2.212(4) . ? Ru C7 2.217(4) . ? Ru C11 2.385(4) . ? Ru Cp1 1.815 . ? Ru Cp2 1.793 . ? Fe C15 2.038(4) . ? Fe C21 2.048(4) . ? Fe C16 2.053(4) . ? Fe C20 2.053(4) . ? Fe C22 2.056(4) . ? Fe C23 2.058(4) . ? Fe C19 2.058(4) . ? Fe C18 2.064(4) . ? Fe C17 2.065(4) . ? Fe C14 2.065(4) . ? Fe C13 3.151(4) . ? Fe Cp3 1.661 . ? Fe Cp4 1.661 . ? C1 C5 1.410(6) . ? C1 C2 1.427(6) . ? C1 H1 1.03(6) . ? C2 C3 1.435(6) . ? C2 H2 0.84(5) . ? C3 C4 1.419(6) . ? C3 H3 0.96(6) . ? C4 C5 1.426(6) . ? C4 H4 0.87(6) . ? C5 H5 0.85(5) . ? C6 C7 1.412(5) . ? C6 C10 1.459(5) . ? C6 H6 0.97(6) . ? C7 C8 1.415(6) . ? C7 H7 0.93(5) . ? C8 C9 1.410(6) . ? C8 H8 0.92(6) . ? C9 C10 1.459(5) . ? C9 H9 1.07(5) . ? C10 C11 1.415(5) . ? C11 C12 1.444(5) . ? C11 H11 1.02(6) . ? C12 C13 1.344(5) . ? C12 H12 1.07(6) . ? C13 C14 1.450(5) . ? C13 H13 1.00(6) . ? C14 C18 1.438(5) . ? C14 C15 1.441(5) . ? C15 C16 1.413(5) . ? C15 H15 1.00(5) . ? C16 C17 1.423(5) . ? C16 H16 0.96(6) . ? C17 C18 1.414(6) . ? C17 H17 0.94(5) . ? C18 H18 0.95(6) . ? C19 C20 1.430(6) . ? C19 C23 1.432(6) . ? C19 H19 0.97(5) . ? C20 C21 1.413(6) . ? C20 H20 1.00(5) . ? C21 C22 1.427(6) . ? C21 H21 0.99(6) . ? C22 C23 1.403(6) . ? C22 H22 0.94(5) . ? C23 H23 0.90(6) . ? P1 F2A 1.53(2) . ? P1 F2A 1.53(2) 7 ? P1 F2 1.600(4) . ? P1 F2 1.600(4) 7 ? P1 F1 1.601(2) 7 ? P1 F1 1.601(2) . ? P1 F3 1.604(3) . ? P1 F3 1.604(3) 7 ? P1 F3A 1.64(3) . ? P1 F3A 1.64(3) 7 ? P2 F6A 1.537(15) 2_655 ? P2 F6A 1.537(15) . ? P2 F5A 1.570(9) 2_655 ? P2 F5A 1.570(9) . ? P2 F6 1.598(12) 2_655 ? P2 F6 1.598(12) . ? P2 F5 1.600(9) 2_655 ? P2 F5 1.600(9) . ? P2 F4 1.602(2) . ? P2 F4 1.602(2) 2_655 ? F6 F6 1.74(6) 2_655 ? F5A F5A 1.63(7) 2_655 ? 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 C10 Ru C3 154.49(15) . . ? C10 Ru C9 40.18(15) . . ? C3 Ru C9 116.79(15) . . ? C10 Ru C6 40.13(14) . . ? C3 Ru C6 156.80(15) . . ? C9 Ru C6 65.84(15) . . ? C10 Ru C2 165.30(15) . . ? C3 Ru C2 38.68(15) . . ? C9 Ru C2 144.40(15) . . ? C6 Ru C2 125.18(15) . . ? C10 Ru C4 129.77(15) . . ? C3 Ru C4 38.21(15) . . ? C9 Ru C4 114.66(15) . . ? C6 Ru C4 164.55(15) . . ? C2 Ru C4 64.28(15) . . ? C10 Ru C5 123.64(15) . . ? C3 Ru C5 63.44(15) . . ? C9 Ru C5 139.73(15) . . ? C6 Ru C5 131.14(15) . . ? C2 Ru C5 63.23(15) . . ? C4 Ru C5 38.13(15) . . ? C10 Ru C8 64.93(15) . . ? C3 Ru C8 103.48(15) . . ? C9 Ru C8 37.61(15) . . ? C6 Ru C8 63.64(15) . . ? C2 Ru C8 111.76(16) . . ? C4 Ru C8 127.07(16) . . ? C5 Ru C8 165.09(15) . . ? C10 Ru C1 138.42(15) . . ? C3 Ru C1 63.82(15) . . ? C9 Ru C1 176.85(15) . . ? C6 Ru C1 114.95(15) . . ? C2 Ru C1 37.98(15) . . ? C4 Ru C1 63.69(15) . . ? C5 Ru C1 37.33(15) . . ? C8 Ru C1 145.54(15) . . ? C10 Ru C7 64.80(14) . . ? C3 Ru C7 120.68(15) . . ? C9 Ru C7 63.52(15) . . ? C6 Ru C7 37.56(14) . . ? C2 Ru C7 103.48(15) . . ? C4 Ru C7 157.69(15) . . ? C5 Ru C7 154.84(15) . . ? C8 Ru C7 37.29(15) . . ? C1 Ru C7 119.11(15) . . ? C10 Ru C11 36.14(13) . . ? C3 Ru C11 137.89(15) . . ? C9 Ru C11 66.05(14) . . ? C6 Ru C11 65.22(14) . . ? C2 Ru C11 148.72(15) . . ? C4 Ru C11 100.34(14) . . ? C5 Ru C11 87.63(14) . . ? C8 Ru C11 99.27(14) . . ? C1 Ru C11 111.29(14) . . ? C7 Ru C11 98.72(14) . . ? Cp1 Ru Cp2 167.8 . . ? C15 Fe C21 116.21(16) . . ? C15 Fe C16 40.42(15) . . ? C21 Fe C16 105.45(17) . . ? C15 Fe C20 105.06(16) . . ? C21 Fe C20 40.29(17) . . ? C16 Fe C20 123.66(17) . . ? C15 Fe C22 151.52(16) . . ? C21 Fe C22 40.69(16) . . ? C16 Fe C22 118.89(16) . . ? C20 Fe C22 68.10(16) . . ? C15 Fe C23 165.16(17) . . ? C21 Fe C23 67.79(17) . . ? C16 Fe C23 154.32(16) . . ? C20 Fe C23 68.14(17) . . ? C22 Fe C23 39.88(16) . . ? C15 Fe C19 125.71(16) . . ? C21 Fe C19 68.13(18) . . ? C16 Fe C19 161.91(17) . . ? C20 Fe C19 40.71(17) . . ? C22 Fe C19 68.04(16) . . ? C23 Fe C19 40.72(16) . . ? C15 Fe C18 68.70(15) . . ? C21 Fe C18 164.47(16) . . ? C16 Fe C18 68.08(15) . . ? C20 Fe C18 155.03(17) . . ? C22 Fe C18 128.80(16) . . ? C23 Fe C18 111.53(16) . . ? C19 Fe C18 122.26(17) . . ? C15 Fe C17 68.08(15) . . ? C21 Fe C17 126.11(17) . . ? C16 Fe C17 40.44(15) . . ? C20 Fe C17 161.84(17) . . ? C22 Fe C17 109.41(16) . . ? C23 Fe C17 122.33(16) . . ? C19 Fe C17 156.67(17) . . ? C18 Fe C17 40.06(15) . . ? C15 Fe C14 41.12(14) . . ? C21 Fe C14 151.73(15) . . ? C16 Fe C14 68.35(15) . . ? C20 Fe C14 118.72(16) . . ? C22 Fe C14 166.51(15) . . ? C23 Fe C14 129.34(16) . . ? C19 Fe C14 108.80(16) . . ? C18 Fe C14 40.77(14) . . ? C17 Fe C14 67.94(15) . . ? Cp3 Fe Cp4 176.8 . . ? C5 C1 C2 107.5(4) . . ? C5 C1 Ru 70.5(2) . . ? C2 C1 Ru 69.4(2) . . ? C5 C1 H1 132(3) . . ? C2 C1 H1 120(3) . . ? Ru C1 H1 125(3) . . ? C1 C2 C3 107.8(4) . . ? C1 C2 Ru 72.6(2) . . ? C3 C2 Ru 70.3(2) . . ? C1 C2 H2 122(4) . . ? C3 C2 H2 129(4) . . ? Ru C2 H2 116(4) . . ? C4 C3 C2 108.2(4) . . ? C4 C3 Ru 71.3(2) . . ? C2 C3 Ru 71.0(2) . . ? C4 C3 H3 130(3) . . ? C2 C3 H3 122(3) . . ? Ru C3 H3 122(3) . . ? C3 C4 C5 107.1(4) . . ? C3 C4 Ru 70.4(2) . . ? C5 C4 Ru 71.6(2) . . ? C3 C4 H4 132(4) . . ? C5 C4 H4 121(4) . . ? Ru C4 H4 123(4) . . ? C1 C5 C4 109.4(4) . . ? C1 C5 Ru 72.1(2) . . ? C4 C5 Ru 70.3(2) . . ? C1 C5 H5 128(4) . . ? C4 C5 H5 123(4) . . ? Ru C5 H5 122(4) . . ? C7 C6 C10 106.8(3) . . ? C7 C6 Ru 73.1(2) . . ? C10 C6 Ru 66.7(2) . . ? C7 C6 H6 126(3) . . ? C10 C6 H6 127(3) . . ? Ru C6 H6 118(3) . . ? C6 C7 C8 109.4(4) . . ? C6 C7 Ru 69.3(2) . . ? C8 C7 Ru 71.0(2) . . ? C6 C7 H7 126(4) . . ? C8 C7 H7 125(4) . . ? Ru C7 H7 125(3) . . ? C9 C8 C7 109.4(4) . . ? C9 C8 Ru 69.4(2) . . ? C7 C8 Ru 71.7(2) . . ? C9 C8 H8 128(3) . . ? C7 C8 H8 123(3) . . ? Ru C8 H8 124(4) . . ? C8 C9 C10 106.9(3) . . ? C8 C9 Ru 73.0(2) . . ? C10 C9 Ru 66.87(19) . . ? C8 C9 H9 129(3) . . ? C10 C9 H9 124(3) . . ? Ru C9 H9 119(3) . . ? C11 C10 C9 119.7(3) . . ? C11 C10 C6 117.7(3) . . ? C9 C10 C6 107.4(3) . . ? C11 C10 Ru 83.8(2) . . ? C9 C10 Ru 72.9(2) . . ? C6 C10 Ru 73.1(2) . . ? C10 C11 C12 124.1(4) . . ? C10 C11 Ru 60.11(19) . . ? C12 C11 Ru 113.9(3) . . ? C10 C11 H11 118(3) . . ? C12 C11 H11 117(3) . . ? Ru C11 H11 106(3) . . ? C13 C12 C11 123.7(4) . . ? C13 C12 H12 118(3) . . ? C11 C12 H12 118(3) . . ? C12 C13 C14 124.5(4) . . ? C12 C13 H13 118(3) . . ? C14 C13 H13 117(3) . . ? C18 C14 C15 107.0(3) . . ? C18 C14 C13 126.3(3) . . ? C15 C14 C13 126.7(3) . . ? C18 C14 Fe 69.6(2) . . ? C15 C14 Fe 68.4(2) . . ? C13 C14 Fe 126.5(3) . . ? C16 C15 C14 108.3(3) . . ? C16 C15 Fe 70.4(2) . . ? C14 C15 Fe 70.5(2) . . ? C16 C15 H15 121(3) . . ? C14 C15 H15 131(3) . . ? Fe C15 H15 124(3) . . ? C15 C16 C17 108.1(3) . . ? C15 C16 Fe 69.2(2) . . ? C17 C16 Fe 70.2(2) . . ? C15 C16 H16 121(3) . . ? C17 C16 H16 131(3) . . ? Fe C16 H16 121(3) . . ? C18 C17 C16 108.6(3) . . ? C18 C17 Fe 69.9(2) . . ? C16 C17 Fe 69.3(2) . . ? C18 C17 H17 126(3) . . ? C16 C17 H17 124(4) . . ? Fe C17 H17 120(3) . . ? C17 C18 C14 108.0(3) . . ? C17 C18 Fe 70.0(2) . . ? C14 C18 Fe 69.7(2) . . ? C17 C18 H18 129(3) . . ? C14 C18 H18 123(3) . . ? Fe C18 H18 129(3) . . ? C20 C19 C23 107.2(4) . . ? C20 C19 Fe 69.5(2) . . ? C23 C19 Fe 69.6(2) . . ? C20 C19 H19 122(3) . . ? C23 C19 H19 130(3) . . ? Fe C19 H19 123(3) . . ? C21 C20 C19 108.0(4) . . ? C21 C20 Fe 69.6(2) . . ? C19 C20 Fe 69.8(2) . . ? C21 C20 H20 123(3) . . ? C19 C20 H20 129(3) . . ? Fe C20 H20 125(3) . . ? C20 C21 C22 108.3(4) . . ? C20 C21 Fe 70.1(2) . . ? C22 C21 Fe 70.0(2) . . ? C20 C21 H21 125(3) . . ? C22 C21 H21 126(3) . . ? Fe C21 H21 124(3) . . ? C23 C22 C21 108.0(4) . . ? C23 C22 Fe 70.2(2) . . ? C21 C22 Fe 69.4(2) . . ? C23 C22 H22 124(3) . . ? C21 C22 H22 128(3) . . ? Fe C22 H22 123(3) . . ? C22 C23 C19 108.5(4) . . ? C22 C23 Fe 70.0(2) . . ? C19 C23 Fe 69.6(2) . . ? C22 C23 H23 123(4) . . ? C19 C23 H23 128(4) . . ? Fe C23 H23 120(4) . . ? F2A P1 F2A 180(2) . 7 ? F2A P1 F2 22.8(11) . . ? F2A P1 F2 157.2(11) 7 . ? F2A P1 F2 157.2(11) . 7 ? F2A P1 F2 22.8(11) 7 7 ? F2 P1 F2 180.0(3) . 7 ? F2A P1 F1 92.7(10) . 7 ? F2A P1 F1 87.3(9) 7 7 ? F2 P1 F1 90.56(14) . 7 ? F2 P1 F1 89.44(14) 7 7 ? F2A P1 F1 87.3(10) . . ? F2A P1 F1 92.7(9) 7 . ? F2 P1 F1 89.44(14) . . ? F2 P1 F1 90.56(14) 7 . ? F1 P1 F1 180.0(2) 7 . ? F2A P1 F3 112.7(12) . . ? F2A P1 F3 67.3(12) 7 . ? F2 P1 F3 90.0(2) . . ? F2 P1 F3 90.0(2) 7 . ? F1 P1 F3 91.43(17) 7 . ? F1 P1 F3 88.57(17) . . ? F2A P1 F3 67.3(12) . 7 ? F2A P1 F3 112.7(12) 7 7 ? F2 P1 F3 90.0(2) . 7 ? F2 P1 F3 90.0(2) 7 7 ? F1 P1 F3 88.57(17) 7 7 ? F1 P1 F3 91.43(17) . 7 ? F3 P1 F3 180.0(6) . 7 ? F2A P1 F3A 89.5(12) . . ? F2A P1 F3A 90.5(12) 7 . ? F2 P1 F3A 66.7(13) . . ? F2 P1 F3A 113.3(13) 7 . ? F1 P1 F3A 79.5(12) 7 . ? F1 P1 F3A 100.5(12) . . ? F3 P1 F3A 26.5(15) . . ? F3 P1 F3A 153.5(15) 7 . ? F2A P1 F3A 90.5(12) . 7 ? F2A P1 F3A 89.5(12) 7 7 ? F2 P1 F3A 113.3(13) . 7 ? F2 P1 F3A 66.7(13) 7 7 ? F1 P1 F3A 100.5(12) 7 7 ? F1 P1 F3A 79.5(12) . 7 ? F3 P1 F3A 153.5(15) . 7 ? F3 P1 F3A 26.5(15) 7 7 ? F3A P1 F3A 180(3) . 7 ? F6A P2 F6A 116(3) 2_655 . ? F6A P2 F5A 91.0(5) 2_655 2_655 ? F6A P2 F5A 153(3) . 2_655 ? F6A P2 F5A 153(3) 2_655 . ? F6A P2 F5A 91.0(5) . . ? F5A P2 F5A 63(3) 2_655 . ? F6A P2 F6 25.2(5) 2_655 2_655 ? F6A P2 F6 91(2) . 2_655 ? F5A P2 F6 115.8(6) 2_655 2_655 ? F5A P2 F6 178(3) . 2_655 ? F6A P2 F6 91(2) 2_655 . ? F6A P2 F6 25.2(5) . . ? F5A P2 F6 178(3) 2_655 . ? F5A P2 F6 115.8(6) . . ? F6 P2 F6 66(2) 2_655 . ? F6A P2 F5 62.9(5) 2_655 2_655 ? F6A P2 F5 177.7(12) . 2_655 ? F5A P2 F5 28.7(5) 2_655 2_655 ? F5A P2 F5 90(3) . 2_655 ? F6 P2 F5 88.1(5) 2_655 2_655 ? F6 P2 F5 153(2) . 2_655 ? F6A P2 F5 177.7(12) 2_655 . ? F6A P2 F5 62.9(5) . . ? F5A P2 F5 90(3) 2_655 . ? F5A P2 F5 28.7(5) . . ? F6 P2 F5 153(2) 2_655 . ? F6 P2 F5 88.1(5) . . ? F5 P2 F5 118(2) 2_655 . ? F6A P2 F4 89.4(5) 2_655 . ? F6A P2 F4 90.3(5) . . ? F5A P2 F4 93.8(7) 2_655 . ? F5A P2 F4 86.6(7) . . ? F6 P2 F4 92.2(6) 2_655 . ? F6 P2 F4 87.5(6) . . ? F5 P2 F4 87.7(4) 2_655 . ? F5 P2 F4 92.6(4) . . ? F6A P2 F4 90.3(5) 2_655 2_655 ? F6A P2 F4 89.4(5) . 2_655 ? F5A P2 F4 86.6(7) 2_655 2_655 ? F5A P2 F4 93.8(7) . 2_655 ? F6 P2 F4 87.5(6) 2_655 2_655 ? F6 P2 F4 92.2(6) . 2_655 ? F5 P2 F4 92.6(4) 2_655 2_655 ? F5 P2 F4 87.7(4) . 2_655 ? F4 P2 F4 179.6(2) . 2_655 ? P2 F6 F6 57.1(11) . 2_655 ? P2 F5A F5A 58.7(13) . 2_655 ? 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 C10 Ru C1 C5 -84.2(3) . . . . ? C3 Ru C1 C5 79.8(3) . . . . ? C9 Ru C1 C5 -22(3) . . . . ? C6 Ru C1 C5 -125.9(2) . . . . ? C2 Ru C1 C5 118.2(3) . . . . ? C4 Ru C1 C5 37.0(2) . . . . ? C8 Ru C1 C5 154.9(3) . . . . ? C7 Ru C1 C5 -168.0(2) . . . . ? C11 Ru C1 C5 -54.3(3) . . . . ? C10 Ru C1 C2 157.6(2) . . . . ? C3 Ru C1 C2 -38.4(2) . . . . ? C9 Ru C1 C2 -140(3) . . . . ? C6 Ru C1 C2 115.9(2) . . . . ? C4 Ru C1 C2 -81.2(3) . . . . ? C5 Ru C1 C2 -118.2(3) . . . . ? C8 Ru C1 C2 36.7(4) . . . . ? C7 Ru C1 C2 73.8(3) . . . . ? C11 Ru C1 C2 -172.5(2) . . . . ? C5 C1 C2 C3 1.3(4) . . . . ? Ru C1 C2 C3 61.9(3) . . . . ? C5 C1 C2 Ru -60.6(3) . . . . ? C10 Ru C2 C1 -84.7(6) . . . . ? C3 Ru C2 C1 116.9(3) . . . . ? C9 Ru C2 C1 176.5(3) . . . . ? C6 Ru C2 C1 -86.3(3) . . . . ? C4 Ru C2 C1 79.5(3) . . . . ? C5 Ru C2 C1 36.8(2) . . . . ? C8 Ru C2 C1 -158.6(2) . . . . ? C7 Ru C2 C1 -120.4(2) . . . . ? C11 Ru C2 C1 13.6(4) . . . . ? C10 Ru C2 C3 158.4(5) . . . . ? C9 Ru C2 C3 59.6(4) . . . . ? C6 Ru C2 C3 156.8(2) . . . . ? C4 Ru C2 C3 -37.4(2) . . . . ? C5 Ru C2 C3 -80.1(3) . . . . ? C8 Ru C2 C3 84.4(3) . . . . ? C1 Ru C2 C3 -116.9(3) . . . . ? C7 Ru C2 C3 122.7(2) . . . . ? C11 Ru C2 C3 -103.3(3) . . . . ? C1 C2 C3 C4 -1.3(4) . . . . ? Ru C2 C3 C4 62.0(3) . . . . ? C1 C2 C3 Ru -63.3(3) . . . . ? C10 Ru C3 C4 74.9(4) . . . . ? C9 Ru C3 C4 96.6(3) . . . . ? C6 Ru C3 C4 -172.6(3) . . . . ? C2 Ru C3 C4 -117.7(3) . . . . ? C5 Ru C3 C4 -38.1(2) . . . . ? C8 Ru C3 C4 134.2(2) . . . . ? C1 Ru C3 C4 -80.0(3) . . . . ? C7 Ru C3 C4 170.2(2) . . . . ? C11 Ru C3 C4 13.4(3) . . . . ? C10 Ru C3 C2 -167.5(3) . . . . ? C9 Ru C3 C2 -145.8(2) . . . . ? C6 Ru C3 C2 -55.0(5) . . . . ? C4 Ru C3 C2 117.7(3) . . . . ? C5 Ru C3 C2 79.5(3) . . . . ? C8 Ru C3 C2 -108.1(3) . . . . ? C1 Ru C3 C2 37.7(2) . . . . ? C7 Ru C3 C2 -72.1(3) . . . . ? C11 Ru C3 C2 131.1(3) . . . . ? C2 C3 C4 C5 0.8(4) . . . . ? Ru C3 C4 C5 62.6(3) . . . . ? C2 C3 C4 Ru -61.8(3) . . . . ? C10 Ru C4 C3 -147.3(2) . . . . ? C9 Ru C4 C3 -102.6(2) . . . . ? C6 Ru C4 C3 169.0(5) . . . . ? C2 Ru C4 C3 37.9(2) . . . . ? C5 Ru C4 C3 116.6(3) . . . . ? C8 Ru C4 C3 -60.8(3) . . . . ? C1 Ru C4 C3 80.4(2) . . . . ? C7 Ru C4 C3 -22.6(5) . . . . ? C11 Ru C4 C3 -170.9(2) . . . . ? C10 Ru C4 C5 96.2(3) . . . . ? C3 Ru C4 C5 -116.6(3) . . . . ? C9 Ru C4 C5 140.8(2) . . . . ? C6 Ru C4 C5 52.5(6) . . . . ? C2 Ru C4 C5 -78.7(3) . . . . ? C8 Ru C4 C5 -177.4(2) . . . . ? C1 Ru C4 C5 -36.2(2) . . . . ? C7 Ru C4 C5 -139.2(4) . . . . ? C11 Ru C4 C5 72.5(2) . . . . ? C2 C1 C5 C4 -0.8(4) . . . . ? Ru C1 C5 C4 -60.7(3) . . . . ? C2 C1 C5 Ru 59.9(3) . . . . ? C3 C4 C5 C1 0.0(4) . . . . ? Ru C4 C5 C1 61.8(3) . . . . ? C3 C4 C5 Ru -61.9(3) . . . . ? C10 Ru C5 C1 127.5(2) . . . . ? C3 Ru C5 C1 -80.9(3) . . . . ? C9 Ru C5 C1 178.2(2) . . . . ? C6 Ru C5 C1 77.2(3) . . . . ? C2 Ru C5 C1 -37.4(2) . . . . ? C4 Ru C5 C1 -119.1(3) . . . . ? C8 Ru C5 C1 -111.1(6) . . . . ? C7 Ru C5 C1 25.2(5) . . . . ? C11 Ru C5 C1 130.8(2) . . . . ? C10 Ru C5 C4 -113.4(3) . . . . ? C3 Ru C5 C4 38.2(2) . . . . ? C9 Ru C5 C4 -62.7(3) . . . . ? C6 Ru C5 C4 -163.7(2) . . . . ? C2 Ru C5 C4 81.7(3) . . . . ? C8 Ru C5 C4 8.0(7) . . . . ? C1 Ru C5 C4 119.1(3) . . . . ? C7 Ru C5 C4 144.3(3) . . . . ? C11 Ru C5 C4 -110.1(2) . . . . ? C10 Ru C6 C7 117.3(3) . . . . ? C3 Ru C6 C7 -24.6(5) . . . . ? C9 Ru C6 C7 77.4(2) . . . . ? C2 Ru C6 C7 -63.3(3) . . . . ? C4 Ru C6 C7 172.8(5) . . . . ? C5 Ru C6 C7 -146.7(2) . . . . ? C8 Ru C6 C7 35.7(2) . . . . ? C1 Ru C6 C7 -106.0(2) . . . . ? C11 Ru C6 C7 150.9(3) . . . . ? C3 Ru C6 C10 -141.9(4) . . . . ? C9 Ru C6 C10 -39.9(2) . . . . ? C2 Ru C6 C10 179.4(2) . . . . ? C4 Ru C6 C10 55.5(6) . . . . ? C5 Ru C6 C10 96.0(3) . . . . ? C8 Ru C6 C10 -81.6(2) . . . . ? C1 Ru C6 C10 136.7(2) . . . . ? C7 Ru C6 C10 -117.3(3) . . . . ? C11 Ru C6 C10 33.7(2) . . . . ? C10 C6 C7 C8 -1.4(4) . . . . ? Ru C6 C7 C8 -59.9(3) . . . . ? C10 C6 C7 Ru 58.5(2) . . . . ? C10 Ru C7 C6 -39.3(2) . . . . ? C3 Ru C7 C6 169.0(2) . . . . ? C9 Ru C7 C6 -84.1(3) . . . . ? C2 Ru C7 C6 131.3(2) . . . . ? C4 Ru C7 C6 -174.9(3) . . . . ? C5 Ru C7 C6 76.7(4) . . . . ? C8 Ru C7 C6 -120.4(3) . . . . ? C1 Ru C7 C6 93.9(3) . . . . ? C11 Ru C7 C6 -26.5(2) . . . . ? C10 Ru C7 C8 81.1(3) . . . . ? C3 Ru C7 C8 -70.6(3) . . . . ? C9 Ru C7 C8 36.2(2) . . . . ? C6 Ru C7 C8 120.4(3) . . . . ? C2 Ru C7 C8 -108.3(2) . . . . ? C4 Ru C7 C8 -54.6(5) . . . . ? C5 Ru C7 C8 -162.9(3) . . . . ? C1 Ru C7 C8 -145.7(2) . . . . ? C11 Ru C7 C8 93.9(2) . . . . ? C6 C7 C8 C9 -0.5(5) . . . . ? Ru C7 C8 C9 -59.4(3) . . . . ? C6 C7 C8 Ru 58.8(3) . . . . ? C10 Ru C8 C9 39.2(2) . . . . ? C3 Ru C8 C9 -116.6(3) . . . . ? C6 Ru C8 C9 84.0(3) . . . . ? C2 Ru C8 C9 -156.4(2) . . . . ? C4 Ru C8 C9 -82.9(3) . . . . ? C5 Ru C8 C9 -89.1(6) . . . . ? C1 Ru C8 C9 -179.7(3) . . . . ? C7 Ru C8 C9 119.9(3) . . . . ? C11 Ru C8 C9 27.7(3) . . . . ? C10 Ru C8 C7 -80.7(2) . . . . ? C3 Ru C8 C7 123.5(2) . . . . ? C9 Ru C8 C7 -119.9(3) . . . . ? C6 Ru C8 C7 -35.9(2) . . . . ? C2 Ru C8 C7 83.7(3) . . . . ? C4 Ru C8 C7 157.2(2) . . . . ? C5 Ru C8 C7 151.0(5) . . . . ? C1 Ru C8 C7 60.4(4) . . . . ? C11 Ru C8 C7 -92.3(2) . . . . ? C7 C8 C9 C10 2.2(4) . . . . ? Ru C8 C9 C10 -58.5(2) . . . . ? C7 C8 C9 Ru 60.8(3) . . . . ? C10 Ru C9 C8 -117.4(3) . . . . ? C3 Ru C9 C8 76.8(3) . . . . ? C6 Ru C9 C8 -77.6(3) . . . . ? C2 Ru C9 C8 39.7(4) . . . . ? C4 Ru C9 C8 119.4(3) . . . . ? C5 Ru C9 C8 156.5(3) . . . . ? C1 Ru C9 C8 177(18) . . . . ? C7 Ru C9 C8 -35.9(2) . . . . ? C11 Ru C9 C8 -149.9(3) . . . . ? C3 Ru C9 C10 -165.7(2) . . . . ? C6 Ru C9 C10 39.9(2) . . . . ? C2 Ru C9 C10 157.1(3) . . . . ? C4 Ru C9 C10 -123.2(2) . . . . ? C5 Ru C9 C10 -86.0(3) . . . . ? C8 Ru C9 C10 117.4(3) . . . . ? C1 Ru C9 C10 -65(3) . . . . ? C7 Ru C9 C10 81.5(2) . . . . ? C11 Ru C9 C10 -32.5(2) . . . . ? C8 C9 C10 C11 134.7(4) . . . . ? Ru C9 C10 C11 72.2(3) . . . . ? C8 C9 C10 C6 -3.1(4) . . . . ? Ru C9 C10 C6 -65.5(2) . . . . ? C8 C9 C10 Ru 62.5(3) . . . . ? C7 C6 C10 C11 -135.9(3) . . . . ? Ru C6 C10 C11 -73.3(3) . . . . ? C7 C6 C10 C9 2.7(4) . . . . ? Ru C6 C10 C9 65.4(2) . . . . ? C7 C6 C10 Ru -62.7(3) . . . . ? C3 Ru C10 C11 -92.9(4) . . . . ? C9 Ru C10 C11 -123.7(3) . . . . ? C6 Ru C10 C11 121.4(3) . . . . ? C2 Ru C10 C11 119.4(6) . . . . ? C4 Ru C10 C11 -42.0(3) . . . . ? C5 Ru C10 C11 5.5(3) . . . . ? C8 Ru C10 C11 -160.4(3) . . . . ? C1 Ru C10 C11 52.0(3) . . . . ? C7 Ru C10 C11 158.2(3) . . . . ? C3 Ru C10 C9 30.8(5) . . . . ? C6 Ru C10 C9 -114.9(3) . . . . ? C2 Ru C10 C9 -116.9(6) . . . . ? C4 Ru C10 C9 81.7(3) . . . . ? C5 Ru C10 C9 129.2(2) . . . . ? C8 Ru C10 C9 -36.7(2) . . . . ? C1 Ru C10 C9 175.7(2) . . . . ? C7 Ru C10 C9 -78.1(2) . . . . ? C11 Ru C10 C9 123.7(3) . . . . ? C3 Ru C10 C6 145.6(3) . . . . ? C9 Ru C10 C6 114.9(3) . . . . ? C2 Ru C10 C6 -2.0(7) . . . . ? C4 Ru C10 C6 -163.4(2) . . . . ? C5 Ru C10 C6 -115.9(2) . . . . ? C8 Ru C10 C6 78.1(2) . . . . ? C1 Ru C10 C6 -69.5(3) . . . . ? C7 Ru C10 C6 36.8(2) . . . . ? C11 Ru C10 C6 -121.4(3) . . . . ? C9 C10 C11 C12 33.8(5) . . . . ? C6 C10 C11 C12 167.3(3) . . . . ? Ru C10 C11 C12 100.1(3) . . . . ? C9 C10 C11 Ru -66.3(3) . . . . ? C6 C10 C11 Ru 67.2(3) . . . . ? C3 Ru C11 C10 140.1(3) . . . . ? C9 Ru C11 C10 36.0(2) . . . . ? C6 Ru C11 C10 -37.3(2) . . . . ? C2 Ru C11 C10 -154.8(3) . . . . ? C4 Ru C11 C10 148.5(2) . . . . ? C5 Ru C11 C10 -175.4(3) . . . . ? C8 Ru C11 C10 17.9(3) . . . . ? C1 Ru C11 C10 -145.9(2) . . . . ? C7 Ru C11 C10 -19.8(3) . . . . ? C10 Ru C11 C12 -116.9(4) . . . . ? C3 Ru C11 C12 23.2(4) . . . . ? C9 Ru C11 C12 -81.0(3) . . . . ? C6 Ru C11 C12 -154.2(3) . . . . ? C2 Ru C11 C12 88.3(4) . . . . ? C4 Ru C11 C12 31.6(3) . . . . ? C5 Ru C11 C12 67.7(3) . . . . ? C8 Ru C11 C12 -99.0(3) . . . . ? C1 Ru C11 C12 97.2(3) . . . . ? C7 Ru C11 C12 -136.8(3) . . . . ? C10 C11 C12 C13 174.7(4) . . . . ? Ru C11 C12 C13 -116.3(4) . . . . ? C11 C12 C13 C14 -176.6(3) . . . . ? C12 C13 C14 C18 173.4(4) . . . . ? C12 C13 C14 C15 -7.5(6) . . . . ? C12 C13 C14 Fe -96.4(4) . . . . ? C15 Fe C14 C18 -118.9(3) . . . . ? C21 Fe C14 C18 -163.5(3) . . . . ? C16 Fe C14 C18 -81.1(2) . . . . ? C20 Fe C14 C18 161.3(2) . . . . ? C22 Fe C14 C18 43.9(7) . . . . ? C23 Fe C14 C18 77.1(3) . . . . ? C19 Fe C14 C18 117.9(2) . . . . ? C17 Fe C14 C18 -37.4(2) . . . . ? C21 Fe C14 C15 -44.6(4) . . . . ? C16 Fe C14 C15 37.8(2) . . . . ? C20 Fe C14 C15 -79.8(3) . . . . ? C22 Fe C14 C15 162.7(6) . . . . ? C23 Fe C14 C15 -164.1(2) . . . . ? C19 Fe C14 C15 -123.2(2) . . . . ? C18 Fe C14 C15 118.9(3) . . . . ? C17 Fe C14 C15 81.5(2) . . . . ? C15 Fe C14 C13 120.5(4) . . . . ? C21 Fe C14 C13 75.9(5) . . . . ? C16 Fe C14 C13 158.2(4) . . . . ? C20 Fe C14 C13 40.7(4) . . . . ? C22 Fe C14 C13 -76.8(7) . . . . ? C23 Fe C14 C13 -43.6(4) . . . . ? C19 Fe C14 C13 -2.7(4) . . . . ? C18 Fe C14 C13 -120.7(4) . . . . ? C17 Fe C14 C13 -158.0(4) . . . . ? C18 C14 C15 C16 -1.4(4) . . . . ? C13 C14 C15 C16 179.3(3) . . . . ? Fe C14 C15 C16 -60.5(3) . . . . ? C18 C14 C15 Fe 59.1(2) . . . . ? C13 C14 C15 Fe -120.2(4) . . . . ? C21 Fe C15 C16 -83.1(3) . . . . ? C20 Fe C15 C16 -124.7(2) . . . . ? C22 Fe C15 C16 -53.0(4) . . . . ? C23 Fe C15 C16 174.6(6) . . . . ? C19 Fe C15 C16 -164.1(2) . . . . ? C18 Fe C15 C16 80.8(2) . . . . ? C17 Fe C15 C16 37.5(2) . . . . ? C14 Fe C15 C16 118.7(3) . . . . ? C21 Fe C15 C14 158.2(2) . . . . ? C16 Fe C15 C14 -118.7(3) . . . . ? C20 Fe C15 C14 116.6(2) . . . . ? C22 Fe C15 C14 -171.7(3) . . . . ? C23 Fe C15 C14 56.0(7) . . . . ? C19 Fe C15 C14 77.3(3) . . . . ? C18 Fe C15 C14 -37.9(2) . . . . ? C17 Fe C15 C14 -81.1(2) . . . . ? C14 C15 C16 C17 0.9(4) . . . . ? Fe C15 C16 C17 -59.7(3) . . . . ? C14 C15 C16 Fe 60.6(3) . . . . ? C21 Fe C16 C15 112.5(2) . . . . ? C20 Fe C16 C15 72.5(3) . . . . ? C22 Fe C16 C15 154.2(2) . . . . ? C23 Fe C16 C15 -176.8(3) . . . . ? C19 Fe C16 C15 45.9(6) . . . . ? C18 Fe C16 C15 -82.5(2) . . . . ? C17 Fe C16 C15 -119.3(3) . . . . ? C14 Fe C16 C15 -38.4(2) . . . . ? C15 Fe C16 C17 119.3(3) . . . . ? C21 Fe C16 C17 -128.2(2) . . . . ? C20 Fe C16 C17 -168.1(2) . . . . ? C22 Fe C16 C17 -86.4(3) . . . . ? C23 Fe C16 C17 -57.5(5) . . . . ? C19 Fe C16 C17 165.3(5) . . . . ? C18 Fe C16 C17 36.9(2) . . . . ? C14 Fe C16 C17 81.0(2) . . . . ? C15 C16 C17 C18 0.0(4) . . . . ? Fe C16 C17 C18 -59.0(3) . . . . ? C15 C16 C17 Fe 59.0(3) . . . . ? C15 Fe C17 C18 82.5(2) . . . . ? C21 Fe C17 C18 -170.3(2) . . . . ? C16 Fe C17 C18 120.1(3) . . . . ? C20 Fe C17 C18 153.4(5) . . . . ? C22 Fe C17 C18 -127.8(2) . . . . ? C23 Fe C17 C18 -85.5(3) . . . . ? C19 Fe C17 C18 -48.5(5) . . . . ? C14 Fe C17 C18 38.0(2) . . . . ? C15 Fe C17 C16 -37.5(2) . . . . ? C21 Fe C17 C16 69.7(3) . . . . ? C20 Fe C17 C16 33.3(6) . . . . ? C22 Fe C17 C16 112.1(2) . . . . ? C23 Fe C17 C16 154.4(2) . . . . ? C19 Fe C17 C16 -168.5(4) . . . . ? C18 Fe C17 C16 -120.1(3) . . . . ? C14 Fe C17 C16 -82.0(2) . . . . ? C16 C17 C18 C14 -0.9(4) . . . . ? Fe C17 C18 C14 -59.5(3) . . . . ? C16 C17 C18 Fe 58.7(3) . . . . ? C15 C14 C18 C17 1.4(4) . . . . ? C13 C14 C18 C17 -179.3(3) . . . . ? Fe C14 C18 C17 59.8(3) . . . . ? C15 C14 C18 Fe -58.4(2) . . . . ? C13 C14 C18 Fe 120.9(4) . . . . ? C15 Fe C18 C17 -80.9(2) . . . . ? C21 Fe C18 C17 30.7(7) . . . . ? C16 Fe C18 C17 -37.2(2) . . . . ? C20 Fe C18 C17 -160.7(3) . . . . ? C22 Fe C18 C17 72.9(3) . . . . ? C23 Fe C18 C17 115.1(2) . . . . ? C19 Fe C18 C17 159.5(2) . . . . ? C14 Fe C18 C17 -119.0(3) . . . . ? C15 Fe C18 C14 38.2(2) . . . . ? C21 Fe C18 C14 149.8(6) . . . . ? C16 Fe C18 C14 81.8(2) . . . . ? C20 Fe C18 C14 -41.6(5) . . . . ? C22 Fe C18 C14 -168.0(2) . . . . ? C23 Fe C18 C14 -125.9(2) . . . . ? C19 Fe C18 C14 -81.5(3) . . . . ? C17 Fe C18 C14 119.0(3) . . . . ? C15 Fe C19 C20 69.8(3) . . . . ? C21 Fe C19 C20 -37.5(2) . . . . ? C16 Fe C19 C20 34.8(6) . . . . ? C22 Fe C19 C20 -81.5(3) . . . . ? C23 Fe C19 C20 -118.4(4) . . . . ? C18 Fe C19 C20 155.5(2) . . . . ? C17 Fe C19 C20 -169.8(4) . . . . ? C14 Fe C19 C20 112.5(2) . . . . ? C15 Fe C19 C23 -171.8(2) . . . . ? C21 Fe C19 C23 80.9(3) . . . . ? C16 Fe C19 C23 153.2(5) . . . . ? C20 Fe C19 C23 118.4(4) . . . . ? C22 Fe C19 C23 36.9(3) . . . . ? C18 Fe C19 C23 -86.1(3) . . . . ? C17 Fe C19 C23 -51.4(5) . . . . ? C14 Fe C19 C23 -129.1(3) . . . . ? C23 C19 C20 C21 -0.3(4) . . . . ? Fe C19 C20 C21 59.4(3) . . . . ? C23 C19 C20 Fe -59.7(3) . . . . ? C15 Fe C20 C21 112.9(2) . . . . ? C16 Fe C20 C21 73.1(3) . . . . ? C22 Fe C20 C21 -37.9(2) . . . . ? C23 Fe C20 C21 -81.0(3) . . . . ? C19 Fe C20 C21 -119.2(3) . . . . ? C18 Fe C20 C21 -175.3(3) . . . . ? C17 Fe C20 C21 47.8(6) . . . . ? C14 Fe C20 C21 155.0(2) . . . . ? C15 Fe C20 C19 -127.9(2) . . . . ? C21 Fe C20 C19 119.2(3) . . . . ? C16 Fe C20 C19 -167.7(2) . . . . ? C22 Fe C20 C19 81.3(3) . . . . ? C23 Fe C20 C19 38.2(2) . . . . ? C18 Fe C20 C19 -56.1(5) . . . . ? C17 Fe C20 C19 166.9(5) . . . . ? C14 Fe C20 C19 -85.8(3) . . . . ? C19 C20 C21 C22 0.2(4) . . . . ? Fe C20 C21 C22 59.8(3) . . . . ? C19 C20 C21 Fe -59.5(3) . . . . ? C15 Fe C21 C20 -82.4(3) . . . . ? C16 Fe C21 C20 -124.3(2) . . . . ? C22 Fe C21 C20 119.2(3) . . . . ? C23 Fe C21 C20 81.9(3) . . . . ? C19 Fe C21 C20 37.9(2) . . . . ? C18 Fe C21 C20 172.6(5) . . . . ? C17 Fe C21 C20 -163.4(2) . . . . ? C14 Fe C21 C20 -51.4(4) . . . . ? C15 Fe C21 C22 158.5(2) . . . . ? C16 Fe C21 C22 116.6(2) . . . . ? C20 Fe C21 C22 -119.2(3) . . . . ? C23 Fe C21 C22 -37.2(2) . . . . ? C19 Fe C21 C22 -81.3(3) . . . . ? C18 Fe C21 C22 53.4(7) . . . . ? C17 Fe C21 C22 77.4(3) . . . . ? C14 Fe C21 C22 -170.5(3) . . . . ? C20 C21 C22 C23 -0.1(4) . . . . ? Fe C21 C22 C23 59.7(3) . . . . ? C20 C21 C22 Fe -59.8(3) . . . . ? C15 Fe C22 C23 -162.8(3) . . . . ? C21 Fe C22 C23 -119.2(3) . . . . ? C16 Fe C22 C23 160.9(2) . . . . ? C20 Fe C22 C23 -81.7(3) . . . . ? C19 Fe C22 C23 -37.6(2) . . . . ? C18 Fe C22 C23 76.8(3) . . . . ? C17 Fe C22 C23 117.6(2) . . . . ? C14 Fe C22 C23 41.3(7) . . . . ? C15 Fe C22 C21 -43.7(4) . . . . ? C16 Fe C22 C21 -79.9(3) . . . . ? C20 Fe C22 C21 37.5(2) . . . . ? C23 Fe C22 C21 119.2(3) . . . . ? C19 Fe C22 C21 81.5(3) . . . . ? C18 Fe C22 C21 -164.0(2) . . . . ? C17 Fe C22 C21 -123.3(2) . . . . ? C14 Fe C22 C21 160.5(6) . . . . ? C21 C22 C23 C19 -0.1(4) . . . . ? Fe C22 C23 C19 59.1(3) . . . . ? C21 C22 C23 Fe -59.2(3) . . . . ? C20 C19 C23 C22 0.2(4) . . . . ? Fe C19 C23 C22 -59.3(3) . . . . ? C20 C19 C23 Fe 59.6(3) . . . . ? C15 Fe C23 C22 146.7(6) . . . . ? C21 Fe C23 C22 37.9(2) . . . . ? C16 Fe C23 C22 -41.4(5) . . . . ? C20 Fe C23 C22 81.6(3) . . . . ? C19 Fe C23 C22 119.8(4) . . . . ? C18 Fe C23 C22 -125.3(2) . . . . ? C17 Fe C23 C22 -81.7(3) . . . . ? C14 Fe C23 C22 -168.5(2) . . . . ? C15 Fe C23 C19 26.9(8) . . . . ? C21 Fe C23 C19 -81.8(3) . . . . ? C16 Fe C23 C19 -161.1(4) . . . . ? C20 Fe C23 C19 -38.2(3) . . . . ? C22 Fe C23 C19 -119.8(4) . . . . ? C18 Fe C23 C19 114.9(3) . . . . ? C17 Fe C23 C19 158.5(3) . . . . ? C14 Fe C23 C19 71.7(3) . . . . ? F6A P2 F6 F6 -4.1(14) 2_655 . . 2_655 ? F6A P2 F6 F6 170(3) . . . 2_655 ? F5A P2 F6 F6 141(24) 2_655 . . 2_655 ? F5A P2 F6 F6 -178.5(14) . . . 2_655 ? F5 P2 F6 F6 -13.8(18) 2_655 . . 2_655 ? F5 P2 F6 F6 173.8(10) . . . 2_655 ? F4 P2 F6 F6 -93.5(10) . . . 2_655 ? F4 P2 F6 F6 86.2(10) 2_655 . . 2_655 ? F6A P2 F5A F5A 14.1(19) 2_655 . . 2_655 ? F6A P2 F5A F5A -173.6(12) . . . 2_655 ? F6 P2 F5A F5A 41(23) 2_655 . . 2_655 ? F6 P2 F5A F5A -178.4(15) . . . 2_655 ? F5 P2 F5A F5A 8.5(14) 2_655 . . 2_655 ? F5 P2 F5A F5A -162(3) . . . 2_655 ? F4 P2 F5A F5A 96.1(14) . . . 2_655 ? F4 P2 F5A F5A -84.1(14) 2_655 . . 2_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.208 _refine_diff_density_min -0.894 _refine_diff_density_rms 0.108 #===END