# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Jose Gimeno' _publ_contact_author_address ; Departamento de Quimica Organica e Inorganica. Facultad de Quimica Universidad de Oviedo C/ Julian Claveria s/n Oviedo 33071 SPAIN ; _publ_contact_author_email 'Prof Jose Gimeno' _publ_section_title ; [Ru(Å3-2-C3H4Me)(CO)(dppf)][SbF6]: A mononuclear 16e- ruthenium(II) catalyst for propargylic substitution and isomerization of HCßCCPh2(OH) ; loop_ _publ_author_name 'Jose Gimeno' 'Victorio Cadierno' 'Josefina Diez' 'Sergio E. Garcia-Garrido' #=============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 245208' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H42 F6 Fe1 N1 O1 P2 Ru1 Sb1' _chemical_formula_sum 'C47 H42 F6 Fe N O P2 Ru Sb' _chemical_formula_weight 1091.43 _chemical_compound_source synthesis 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' N N 0.0061 0.0033 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _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 10.884(11) _cell_length_b 30.69(6) _cell_length_c 13.706(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.55(3) _cell_angle_gamma 90.00 _cell_volume 4431(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 18 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.297 _exptl_crystal_size_mid 0.132 _exptl_crystal_size_min 0.132 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 1.399 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ; Nonius CAD4 single crystal diffractometer. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD4' _diffrn_measurement_method \w-2\Q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 7.10 _diffrn_reflns_number 9152 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.1376 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.99 _reflns_number_total 8687 _reflns_number_gt 4626 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Nonius CAD-4 Diffractometer Control Sofware. Data collection with profile analysis over all reflections (Lehman and Larsen, 1974; Grant and Gabe, 1978) ; _computing_cell_refinement 'CRYSDA (Beurskens et al, 1996)' _computing_data_reduction 'THE REFLEX (local program)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^+6.0777P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8687 _refine_ls_number_parameters 657 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1775 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1712 _refine_ls_wR_factor_gt 0.1326 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4596(9) 0.1435(3) 0.1637(8) 0.052(3) Uani 1 1 d . . . H1A H 0.4891 0.1677 0.2090 0.063 Uiso 1 1 calc R . . H1B H 0.5260 0.1229 0.1603 0.063 Uiso 1 1 calc R . . C2 C 0.3721(9) 0.1534(3) 0.0725(7) 0.049(2) Uani 1 1 d . . . C3 C 0.2627(10) 0.1764(3) 0.0699(8) 0.048(3) Uani 1 1 d . . . C4 C 0.3931(10) 0.1348(4) -0.0249(7) 0.062(3) Uani 1 1 d . . . H4A H 0.4729 0.1197 -0.0108 0.092 Uiso 1 1 calc R . . H4B H 0.3939 0.1580 -0.0715 0.092 Uiso 1 1 calc R . . H4C H 0.3258 0.1148 -0.0537 0.092 Uiso 1 1 calc R . . C5 C 0.2761(8) 0.1593(3) 0.2759(7) 0.037(2) Uani 1 1 d . . . C6 C 0.2938(10) 0.2232(3) 0.4039(8) 0.061(3) Uani 1 1 d . . . H6A H 0.2760 0.2136 0.4664 0.073 Uiso 1 1 calc R . . H6B H 0.2325 0.2456 0.3748 0.073 Uiso 1 1 calc R . . C7 C 0.4251(9) 0.2419(3) 0.4256(8) 0.053(3) Uani 1 1 d . . . C8 C 0.4746(11) 0.2563(4) 0.3502(9) 0.074(3) Uani 1 1 d . . . H8 H 0.4272 0.2535 0.2839 0.089 Uiso 1 1 calc R . . C9 C 0.5929(14) 0.2749(5) 0.3691(13) 0.114(6) Uani 1 1 d . . . H9 H 0.6243 0.2849 0.3159 0.137 Uiso 1 1 calc R . . C10 C 0.6633(14) 0.2787(6) 0.4643(18) 0.130(7) Uani 1 1 d . . . H10 H 0.7458 0.2894 0.4772 0.156 Uiso 1 1 calc R . . C11 C 0.6125(14) 0.2667(6) 0.5429(14) 0.120(6) Uani 1 1 d . . . H11 H 0.6577 0.2718 0.6091 0.144 Uiso 1 1 calc R . . C12 C 0.4936(12) 0.2470(4) 0.5233(9) 0.078(4) Uani 1 1 d . . . H12 H 0.4611 0.2373 0.5761 0.094 Uiso 1 1 calc R . . C13 C 0.2714(9) 0.0392(3) 0.3689(6) 0.045(2) Uani 1 1 d . . . C14 C 0.1982(9) 0.0651(4) 0.4197(7) 0.050(2) Uani 1 1 d . . . C15 C 0.1357(10) 0.0379(5) 0.4733(8) 0.065(3) Uani 1 1 d . . . C16 C 0.1679(10) -0.0050(5) 0.4569(9) 0.069(4) Uani 1 1 d . . . C17 C 0.2520(10) -0.0048(4) 0.3925(9) 0.059(3) Uani 1 1 d . . . C18 C -0.0018(8) 0.0576(3) 0.1971(6) 0.038(2) Uani 1 1 d . . . C19 C -0.0892(9) 0.0486(4) 0.2567(8) 0.054(3) Uani 1 1 d . . . C20 C -0.0987(12) 0.0045(4) 0.2691(9) 0.068(3) Uani 1 1 d . . . C21 C -0.0228(12) -0.0174(4) 0.2156(8) 0.062(3) Uani 1 1 d . . . C22 C 0.0389(11) 0.0153(3) 0.1717(8) 0.056(3) Uani 1 1 d . . . C23 C -0.0118(8) 0.1531(3) 0.2104(7) 0.040(2) Uani 1 1 d . . . C24 C -0.0227(11) 0.1533(4) 0.3087(9) 0.055(3) Uani 1 1 d . . . C25 C -0.0583(12) 0.1902(4) 0.3521(10) 0.068(3) Uani 1 1 d . . . C26 C -0.0803(13) 0.2270(5) 0.3020(12) 0.077(4) Uani 1 1 d . . . C27 C -0.0671(11) 0.2290(4) 0.2051(12) 0.073(4) Uani 1 1 d . . . C28 C -0.0370(10) 0.1919(3) 0.1571(9) 0.058(3) Uani 1 1 d . . . C29 C -0.0596(8) 0.1078(3) 0.0227(6) 0.043(2) Uani 1 1 d . . . C30 C -0.0248(10) 0.1232(4) -0.0609(7) 0.059(3) Uani 1 1 d . . . H30 H 0.0574 0.1330 -0.0558 0.071 Uiso 1 1 calc R . . C31 C -0.1144(13) 0.1236(5) -0.1527(9) 0.075(4) Uani 1 1 d . . . C32 C -0.2317(12) 0.1080(4) -0.1661(9) 0.074(4) Uani 1 1 d . . . C33 C -0.2665(12) 0.0928(6) -0.0819(11) 0.105(6) Uani 1 1 d . . . C34 C -0.1815(10) 0.0923(5) 0.0097(9) 0.078(4) Uani 1 1 d . . . C35 C 0.4958(8) 0.0918(3) 0.3916(6) 0.0339(19) Uani 1 1 d . . . C36 C 0.6168(10) 0.0940(3) 0.3793(8) 0.053(3) Uani 1 1 d . . . C37 C 0.7127(10) 0.1154(4) 0.4502(9) 0.064(3) Uani 1 1 d . . . C38 C 0.6868(12) 0.1342(5) 0.5309(11) 0.072(4) Uani 1 1 d . . . C39 C 0.5676(12) 0.1317(4) 0.5461(9) 0.063(3) Uani 1 1 d . . . C40 C 0.4742(11) 0.1102(4) 0.4777(8) 0.053(3) Uani 1 1 d . . . C41 C 0.4593(8) 0.0199(3) 0.2591(6) 0.037(2) Uani 1 1 d . . . C42 C 0.4874(10) 0.0192(4) 0.1668(7) 0.048(3) Uani 1 1 d . . . C43 C 0.5647(11) -0.0125(4) 0.1414(8) 0.058(3) Uani 1 1 d . . . C44 C 0.6094(10) -0.0449(4) 0.2092(8) 0.057(3) Uani 1 1 d . . . C45 C 0.5857(10) -0.0445(3) 0.3022(9) 0.053(3) Uani 1 1 d . . . C46 C 0.5110(9) -0.0125(3) 0.3279(8) 0.047(2) Uani 1 1 d . . . C47 C 0.2424(8) 0.0730(3) 0.0611(7) 0.042(2) Uani 1 1 d . . . F1 F -0.0097(7) 0.1708(2) 0.6216(6) 0.094(2) Uani 1 1 d . . . F2 F 0.1370(8) 0.1071(2) 0.6996(7) 0.122(3) Uani 1 1 d . . . F3 F 0.1741(9) 0.1481(3) 0.5392(6) 0.130(3) Uani 1 1 d . . . F4 F 0.3370(7) 0.1557(3) 0.7122(6) 0.107(3) Uani 1 1 d . . . F5 F 0.1890(8) 0.2212(2) 0.6365(6) 0.106(3) Uani 1 1 d . . . F6 F 0.1525(8) 0.1819(3) 0.7943(5) 0.107(3) Uani 1 1 d . . . Fe1 Fe 0.08465(12) 0.02449(4) 0.32234(9) 0.0407(3) Uani 1 1 d . . . N1 N 0.2811(7) 0.1867(2) 0.3347(6) 0.0454(19) Uani 1 1 d . . . P1 P 0.3682(2) 0.06521(7) 0.29392(16) 0.0324(5) Uani 1 1 d . . . P2 P 0.0489(2) 0.10790(7) 0.15028(16) 0.0350(5) Uani 1 1 d . . . Ru1 Ru 0.26899(6) 0.11510(2) 0.16517(5) 0.03179(18) Uani 1 1 d . . . Sb1 Sb 0.16165(7) 0.16404(2) 0.66681(5) 0.0547(2) Uani 1 1 d . . . O1 O 0.2202(7) 0.0468(2) -0.0002(5) 0.0617(19) Uani 1 1 d . . . H25 H -0.075(7) 0.190(2) 0.411(6) 0.03(2) Uiso 1 1 d . . . H24 H -0.028(8) 0.132(3) 0.333(6) 0.03(3) Uiso 1 1 d . . . H34 H -0.206(8) 0.081(3) 0.063(6) 0.04(3) Uiso 1 1 d . . . H3A H 0.271(6) 0.201(2) 0.123(5) 0.005(15) Uiso 1 1 d . . . H14 H 0.189(8) 0.101(3) 0.410(6) 0.05(3) Uiso 1 1 d . . . H45 H 0.629(7) -0.062(2) 0.348(6) 0.03(2) Uiso 1 1 d . . . H19 H -0.132(7) 0.069(2) 0.277(5) 0.02(2) Uiso 1 1 d . . . H16 H 0.153(11) -0.035(4) 0.474(8) 0.09(4) Uiso 1 1 d . . . H31 H -0.088(6) 0.134(2) -0.197(5) 0.008(18) Uiso 1 1 d . . . H40 H 0.413(8) 0.112(3) 0.492(6) 0.03(3) Uiso 1 1 d . . . H28 H -0.008(9) 0.194(3) 0.087(7) 0.06(3) Uiso 1 1 d . . . H3B H 0.196(7) 0.185(2) 0.015(6) 0.03(2) Uiso 1 1 d . . . H38 H 0.738(9) 0.141(3) 0.577(7) 0.05(3) Uiso 1 1 d . . . H46 H 0.492(8) -0.014(3) 0.382(6) 0.04(3) Uiso 1 1 d . . . H20 H -0.143(8) -0.009(3) 0.307(6) 0.04(3) Uiso 1 1 d . . . H36 H 0.635(8) 0.081(3) 0.321(6) 0.04(2) Uiso 1 1 d . . . H33 H -0.341(11) 0.083(4) -0.083(8) 0.08(4) Uiso 1 1 d . . . H27 H -0.074(7) 0.250(3) 0.167(6) 0.02(2) Uiso 1 1 d . . . H39 H 0.566(9) 0.138(3) 0.606(7) 0.06(3) Uiso 1 1 d . . . H37 H 0.790(9) 0.115(3) 0.444(6) 0.05(3) Uiso 1 1 d . . . H42 H 0.476(7) 0.038(2) 0.124(6) 0.03(2) Uiso 1 1 d . . . H43 H 0.589(11) -0.014(4) 0.084(9) 0.11(5) Uiso 1 1 d . . . H17 H 0.285(7) -0.028(2) 0.370(5) 0.02(2) Uiso 1 1 d . . . H21 H 0.004(10) -0.051(3) 0.207(7) 0.08(3) Uiso 1 1 d . . . H22 H 0.106(9) 0.009(3) 0.148(7) 0.06(3) Uiso 1 1 d . . . H32 H -0.301(11) 0.110(4) -0.238(9) 0.10(4) Uiso 1 1 d . . . H15 H 0.065(10) 0.049(3) 0.512(8) 0.09(4) Uiso 1 1 d . . . H44 H 0.652(7) -0.065(2) 0.199(5) 0.02(2) Uiso 1 1 d . . . H26 H -0.104(11) 0.251(4) 0.336(9) 0.10(4) 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 C1 0.034(5) 0.058(6) 0.067(7) -0.004(5) 0.016(5) -0.018(5) C2 0.043(6) 0.054(6) 0.053(6) 0.005(5) 0.018(5) -0.015(5) C3 0.052(7) 0.040(6) 0.048(6) 0.022(5) 0.008(5) 0.002(5) C4 0.066(8) 0.072(7) 0.053(7) 0.007(5) 0.028(6) 0.000(6) C5 0.025(5) 0.039(5) 0.046(5) 0.004(4) 0.004(4) -0.001(4) C6 0.062(7) 0.057(7) 0.068(7) -0.027(5) 0.022(6) -0.018(6) C7 0.049(6) 0.041(6) 0.064(7) -0.025(5) 0.004(5) -0.002(5) C8 0.052(7) 0.092(9) 0.072(8) -0.014(7) 0.003(6) -0.017(7) C9 0.074(10) 0.154(16) 0.119(13) -0.031(12) 0.032(10) -0.042(11) C10 0.047(9) 0.143(16) 0.19(2) -0.062(15) 0.016(12) -0.023(10) C11 0.061(10) 0.137(15) 0.134(15) -0.057(12) -0.030(10) 0.014(10) C12 0.067(8) 0.085(9) 0.070(8) -0.011(7) -0.005(7) 0.009(7) C13 0.039(5) 0.060(6) 0.035(5) 0.003(4) 0.006(4) 0.005(5) C14 0.041(6) 0.070(7) 0.037(5) -0.004(5) 0.006(4) -0.018(5) C15 0.041(6) 0.108(10) 0.046(6) 0.013(6) 0.013(5) -0.006(7) C16 0.038(6) 0.090(10) 0.072(8) 0.045(7) 0.000(6) -0.012(6) C17 0.044(6) 0.051(7) 0.084(8) 0.025(6) 0.018(6) 0.013(5) C18 0.025(5) 0.048(5) 0.039(5) 0.005(4) 0.004(4) -0.006(4) C19 0.035(6) 0.076(8) 0.055(7) 0.006(6) 0.016(5) 0.008(6) C20 0.067(8) 0.070(8) 0.062(8) 0.019(6) 0.006(6) -0.031(7) C21 0.084(9) 0.046(6) 0.052(6) -0.006(5) 0.009(6) -0.027(6) C22 0.063(8) 0.050(6) 0.056(7) -0.001(5) 0.015(6) -0.013(6) C23 0.029(5) 0.044(5) 0.047(5) 0.003(4) 0.012(4) 0.002(4) C24 0.064(8) 0.045(7) 0.060(7) -0.003(6) 0.021(6) 0.004(6) C25 0.081(9) 0.068(8) 0.060(8) -0.007(6) 0.028(7) 0.012(7) C26 0.076(9) 0.065(9) 0.091(10) -0.023(8) 0.024(8) -0.002(7) C27 0.059(8) 0.046(7) 0.105(11) 0.013(8) 0.005(8) 0.006(6) C28 0.047(6) 0.054(7) 0.069(7) 0.005(6) 0.010(6) 0.006(5) C29 0.031(5) 0.053(6) 0.043(5) -0.003(4) 0.007(4) -0.004(4) C30 0.042(6) 0.091(8) 0.041(6) 0.002(5) 0.003(5) 0.005(6) C31 0.077(9) 0.102(10) 0.048(7) 0.020(7) 0.019(7) -0.002(8) C32 0.062(8) 0.097(10) 0.049(7) 0.001(7) -0.014(6) 0.001(7) C33 0.041(8) 0.185(17) 0.068(9) 0.020(9) -0.024(7) -0.039(9) C34 0.033(6) 0.137(12) 0.055(7) 0.019(8) -0.005(5) -0.025(7) C35 0.029(5) 0.034(5) 0.034(5) 0.001(4) -0.001(4) 0.000(4) C36 0.044(6) 0.067(7) 0.049(6) -0.012(5) 0.011(5) -0.009(5) C37 0.031(6) 0.087(9) 0.072(8) -0.002(7) 0.006(6) -0.013(6) C38 0.048(8) 0.092(10) 0.064(9) 0.000(7) -0.009(7) -0.027(7) C39 0.060(8) 0.077(8) 0.044(7) -0.005(6) 0.001(6) -0.003(6) C40 0.041(6) 0.070(8) 0.044(6) -0.017(5) 0.005(5) -0.002(6) C41 0.027(5) 0.050(5) 0.031(4) 0.001(4) -0.002(4) 0.006(4) C42 0.050(6) 0.056(7) 0.036(6) 0.011(5) 0.003(5) 0.007(5) C43 0.061(7) 0.073(8) 0.040(6) -0.014(6) 0.010(5) 0.021(6) C44 0.055(7) 0.056(7) 0.050(7) -0.016(6) -0.007(5) 0.023(6) C45 0.045(6) 0.043(6) 0.062(7) 0.009(5) -0.003(5) 0.010(5) C46 0.037(6) 0.049(6) 0.055(7) 0.013(5) 0.014(5) 0.011(5) C47 0.024(5) 0.056(6) 0.042(5) -0.001(5) 0.001(4) 0.003(4) F1 0.073(5) 0.089(5) 0.109(6) -0.014(4) 0.002(4) -0.003(4) F2 0.126(7) 0.062(5) 0.188(9) 0.036(5) 0.056(6) 0.017(5) F3 0.188(10) 0.124(7) 0.088(6) -0.035(5) 0.053(6) 0.016(7) F4 0.066(5) 0.115(6) 0.135(7) -0.007(5) 0.015(5) 0.015(4) F5 0.141(7) 0.052(4) 0.143(7) 0.016(4) 0.073(6) 0.010(4) F6 0.123(7) 0.140(7) 0.059(4) -0.003(4) 0.026(4) 0.011(5) Fe1 0.0350(8) 0.0440(8) 0.0422(7) 0.0058(6) 0.0079(6) -0.0069(6) N1 0.041(5) 0.046(5) 0.046(5) -0.012(4) 0.005(4) -0.007(4) P1 0.0294(12) 0.0363(12) 0.0312(11) 0.0009(9) 0.0070(10) -0.0002(10) P2 0.0290(12) 0.0395(13) 0.0345(12) 0.0000(10) 0.0045(10) -0.0003(10) Ru1 0.0285(4) 0.0339(4) 0.0323(4) 0.0001(3) 0.0063(3) -0.0016(3) Sb1 0.0659(5) 0.0484(4) 0.0528(4) 0.0002(3) 0.0203(4) 0.0034(4) O1 0.059(5) 0.072(5) 0.052(4) -0.026(4) 0.009(4) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.402(13) . ? C1 Ru1 2.255(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.378(13) . ? C2 C4 1.520(13) . ? C2 Ru1 2.229(9) . ? C3 Ru1 2.282(9) . ? C3 H3A 1.03(6) . ? C3 H3B 0.95(8) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 N1 1.156(10) . ? C5 Ru1 2.022(9) . ? C6 N1 1.453(11) . ? C6 C7 1.499(13) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.354(15) . ? C7 C12 1.368(14) . ? C8 C9 1.373(16) . ? C8 H8 0.9300 . ? C9 C10 1.34(2) . ? C9 H9 0.9300 . ? C10 C11 1.38(2) . ? C10 H10 0.9300 . ? C11 C12 1.392(18) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C17 1.416(13) . ? C13 C14 1.423(13) . ? C13 P1 1.830(9) . ? C13 Fe1 2.023(9) . ? C14 C15 1.396(14) . ? C14 Fe1 2.007(9) . ? C14 H14 1.12(8) . ? C15 C16 1.396(17) . ? C15 Fe1 2.046(11) . ? C15 H15 1.09(10) . ? C16 C17 1.422(15) . ? C16 Fe1 2.049(11) . ? C16 H16 0.98(11) . ? C17 Fe1 2.042(10) . ? C17 H17 0.89(7) . ? C18 C19 1.429(12) . ? C18 C22 1.442(14) . ? C18 P2 1.810(9) . ? C18 Fe1 2.014(8) . ? C19 C20 1.372(15) . ? C19 Fe1 2.021(11) . ? C19 H19 0.86(7) . ? C20 C21 1.405(16) . ? C20 Fe1 2.040(12) . ? C20 H20 0.90(8) . ? C21 C22 1.422(14) . ? C21 Fe1 2.074(10) . ? C21 H21 1.09(10) . ? C22 Fe1 2.018(11) . ? C22 H22 0.89(9) . ? C23 C24 1.382(13) . ? C23 C28 1.388(13) . ? C23 P2 1.821(9) . ? C24 C25 1.379(15) . ? C24 H24 0.75(7) . ? C25 C26 1.312(17) . ? C25 H25 0.87(8) . ? C26 C27 1.372(18) . ? C26 H26 0.95(12) . ? C27 C28 1.395(16) . ? C27 H27 0.81(7) . ? C28 H28 1.09(9) . ? C29 C30 1.377(12) . ? C29 C34 1.379(13) . ? C29 P2 1.848(9) . ? C30 C31 1.385(15) . ? C30 H30 0.9300 . ? C31 C32 1.333(17) . ? C31 H31 0.81(6) . ? C32 C33 1.382(18) . ? C32 H32 1.08(12) . ? C33 C34 1.360(15) . ? C33 H33 0.86(11) . ? C34 H34 0.91(8) . ? C35 C36 1.371(12) . ? C35 C40 1.381(13) . ? C35 P1 1.858(8) . ? C36 C37 1.398(14) . ? C36 H36 0.96(8) . ? C37 C38 1.340(17) . ? C37 H37 0.86(9) . ? C38 C39 1.367(16) . ? C38 H38 0.76(9) . ? C39 C40 1.366(15) . ? C39 H39 0.85(9) . ? C40 H40 0.74(7) . ? C41 C42 1.375(12) . ? C41 C46 1.389(12) . ? C41 P1 1.839(9) . ? C42 C43 1.388(14) . ? C42 H42 0.81(7) . ? C43 C44 1.365(15) . ? C43 H43 0.90(12) . ? C44 C45 1.363(14) . ? C44 H44 0.81(7) . ? C45 C46 1.375(14) . ? C45 H45 0.86(7) . ? C46 H46 0.82(8) . ? C47 O1 1.144(10) . ? C47 Ru1 1.891(10) . ? F1 Sb1 1.824(7) . ? F2 Sb1 1.841(8) . ? F3 Sb1 1.854(7) . ? F4 Sb1 1.870(7) . ? F5 Sb1 1.844(7) . ? F6 Sb1 1.857(7) . ? P1 Ru1 2.381(3) . ? P2 Ru1 2.362(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Ru1 70.8(5) . . ? C2 C1 H1A 116.5 . . ? Ru1 C1 H1A 116.5 . . ? C2 C1 H1B 116.5 . . ? Ru1 C1 H1B 116.5 . . ? H1A C1 H1B 113.5 . . ? C3 C2 C1 121.6(9) . . ? C3 C2 C4 119.4(9) . . ? C1 C2 C4 118.8(9) . . ? C3 C2 Ru1 74.3(5) . . ? C1 C2 Ru1 72.8(5) . . ? C4 C2 Ru1 120.7(7) . . ? C2 C3 Ru1 70.1(5) . . ? C2 C3 H3A 115(3) . . ? Ru1 C3 H3A 102(3) . . ? C2 C3 H3B 131(5) . . ? Ru1 C3 H3B 127(5) . . ? H3A C3 H3B 105(6) . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 Ru1 175.4(8) . . ? N1 C6 C7 110.8(8) . . ? N1 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C12 119.1(11) . . ? C8 C7 C6 121.0(10) . . ? C12 C7 C6 119.7(11) . . ? C7 C8 C9 121.8(12) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C10 C9 C8 119.9(16) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 119.6(15) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C12 120.1(15) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C7 C12 C11 119.3(14) . . ? C7 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C17 C13 C14 106.6(9) . . ? C17 C13 P1 133.1(8) . . ? C14 C13 P1 120.2(7) . . ? C17 C13 Fe1 70.3(6) . . ? C14 C13 Fe1 68.7(5) . . ? P1 C13 Fe1 126.5(5) . . ? C15 C14 C13 109.4(10) . . ? C15 C14 Fe1 71.4(6) . . ? C13 C14 Fe1 69.9(6) . . ? C15 C14 H14 128(4) . . ? C13 C14 H14 123(4) . . ? Fe1 C14 H14 121(4) . . ? C14 C15 C16 107.6(10) . . ? C14 C15 Fe1 68.4(6) . . ? C16 C15 Fe1 70.2(7) . . ? C14 C15 H15 125(6) . . ? C16 C15 H15 127(6) . . ? Fe1 C15 H15 121(6) . . ? C15 C16 C17 108.8(10) . . ? C15 C16 Fe1 69.9(6) . . ? C17 C16 Fe1 69.4(6) . . ? C15 C16 H16 142(7) . . ? C17 C16 H16 109(7) . . ? Fe1 C16 H16 125(7) . . ? C13 C17 C16 107.6(10) . . ? C13 C17 Fe1 68.9(6) . . ? C16 C17 Fe1 69.9(6) . . ? C13 C17 H17 126(5) . . ? C16 C17 H17 126(5) . . ? Fe1 C17 H17 125(5) . . ? C19 C18 C22 104.6(9) . . ? C19 C18 P2 132.4(8) . . ? C22 C18 P2 122.9(7) . . ? C19 C18 Fe1 69.5(5) . . ? C22 C18 Fe1 69.2(6) . . ? P2 C18 Fe1 127.9(5) . . ? C20 C19 C18 110.1(10) . . ? C20 C19 Fe1 71.0(7) . . ? C18 C19 Fe1 69.0(5) . . ? C20 C19 H19 128(5) . . ? C18 C19 H19 122(5) . . ? Fe1 C19 H19 130(5) . . ? C19 C20 C21 109.6(10) . . ? C19 C20 Fe1 69.5(6) . . ? C21 C20 Fe1 71.3(7) . . ? C19 C20 H20 127(6) . . ? C21 C20 H20 123(6) . . ? Fe1 C20 H20 124(6) . . ? C20 C21 C22 106.6(10) . . ? C20 C21 Fe1 68.7(6) . . ? C22 C21 Fe1 67.6(6) . . ? C20 C21 H21 136(5) . . ? C22 C21 H21 117(5) . . ? Fe1 C21 H21 123(6) . . ? C21 C22 C18 109.1(10) . . ? C21 C22 Fe1 71.8(6) . . ? C18 C22 Fe1 68.9(6) . . ? C21 C22 H22 122(6) . . ? C18 C22 H22 127(6) . . ? Fe1 C22 H22 113(6) . . ? C24 C23 C28 117.1(9) . . ? C24 C23 P2 125.1(7) . . ? C28 C23 P2 117.5(7) . . ? C25 C24 C23 121.8(11) . . ? C25 C24 H24 119(7) . . ? C23 C24 H24 117(7) . . ? C26 C25 C24 121.0(13) . . ? C26 C25 H25 116(5) . . ? C24 C25 H25 122(5) . . ? C25 C26 C27 119.7(13) . . ? C25 C26 H26 117(7) . . ? C27 C26 H26 123(7) . . ? C26 C27 C28 120.9(12) . . ? C26 C27 H27 130(6) . . ? C28 C27 H27 109(6) . . ? C23 C28 C27 119.4(11) . . ? C23 C28 H28 117(5) . . ? C27 C28 H28 122(5) . . ? C30 C29 C34 117.9(9) . . ? C30 C29 P2 122.9(7) . . ? C34 C29 P2 119.2(7) . . ? C29 C30 C31 118.8(10) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? C32 C31 C30 123.6(12) . . ? C32 C31 H31 124(5) . . ? C30 C31 H31 113(5) . . ? C31 C32 C33 117.4(11) . . ? C31 C32 H32 122(6) . . ? C33 C32 H32 121(6) . . ? C34 C33 C32 120.6(12) . . ? C34 C33 H33 115(8) . . ? C32 C33 H33 124(8) . . ? C33 C34 C29 121.6(12) . . ? C33 C34 H34 119(6) . . ? C29 C34 H34 120(6) . . ? C36 C35 C40 117.4(9) . . ? C36 C35 P1 120.0(7) . . ? C40 C35 P1 122.6(7) . . ? C35 C36 C37 120.7(10) . . ? C35 C36 H36 119(5) . . ? C37 C36 H36 120(5) . . ? C38 C37 C36 120.1(11) . . ? C38 C37 H37 120(6) . . ? C36 C37 H37 120(6) . . ? C37 C38 C39 120.4(12) . . ? C37 C38 H38 123(8) . . ? C39 C38 H38 115(8) . . ? C40 C39 C38 119.7(12) . . ? C40 C39 H39 125(7) . . ? C38 C39 H39 113(7) . . ? C39 C40 C35 121.8(11) . . ? C39 C40 H40 110(7) . . ? C35 C40 H40 128(7) . . ? C42 C41 C46 118.0(9) . . ? C42 C41 P1 120.6(7) . . ? C46 C41 P1 121.2(7) . . ? C41 C42 C43 122.0(10) . . ? C41 C42 H42 129(6) . . ? C43 C42 H42 108(6) . . ? C44 C43 C42 118.4(10) . . ? C44 C43 H43 116(8) . . ? C42 C43 H43 125(8) . . ? C45 C44 C43 120.8(10) . . ? C45 C44 H44 115(5) . . ? C43 C44 H44 124(5) . . ? C44 C45 C46 120.6(10) . . ? C44 C45 H45 118(5) . . ? C46 C45 H45 120(5) . . ? C45 C46 C41 120.1(10) . . ? C45 C46 H46 119(6) . . ? C41 C46 H46 120(6) . . ? O1 C47 Ru1 176.0(8) . . ? C14 Fe1 C18 109.3(4) . . ? C14 Fe1 C22 136.0(4) . . ? C18 Fe1 C22 41.9(4) . . ? C14 Fe1 C19 114.8(5) . . ? C18 Fe1 C19 41.5(4) . . ? C22 Fe1 C19 68.5(5) . . ? C14 Fe1 C13 41.4(4) . . ? C18 Fe1 C13 111.9(3) . . ? C22 Fe1 C13 108.9(4) . . ? C19 Fe1 C13 144.4(4) . . ? C14 Fe1 C20 143.9(5) . . ? C18 Fe1 C20 69.0(4) . . ? C22 Fe1 C20 67.9(5) . . ? C19 Fe1 C20 39.5(4) . . ? C13 Fe1 C20 174.5(5) . . ? C14 Fe1 C17 68.4(5) . . ? C18 Fe1 C17 142.6(4) . . ? C22 Fe1 C17 112.5(5) . . ? C19 Fe1 C17 174.7(4) . . ? C13 Fe1 C17 40.8(4) . . ? C20 Fe1 C17 135.5(5) . . ? C14 Fe1 C15 40.3(4) . . ? C18 Fe1 C15 135.3(5) . . ? C22 Fe1 C15 176.0(5) . . ? C19 Fe1 C15 111.2(5) . . ? C13 Fe1 C15 68.9(4) . . ? C20 Fe1 C15 114.6(5) . . ? C17 Fe1 C15 68.2(5) . . ? C14 Fe1 C16 67.4(5) . . ? C18 Fe1 C16 175.0(5) . . ? C22 Fe1 C16 143.0(6) . . ? C19 Fe1 C16 135.6(4) . . ? C13 Fe1 C16 68.4(4) . . ? C20 Fe1 C16 111.2(4) . . ? C17 Fe1 C16 40.7(4) . . ? C15 Fe1 C16 39.9(5) . . ? C14 Fe1 C21 175.8(4) . . ? C18 Fe1 C21 69.6(4) . . ? C22 Fe1 C21 40.7(4) . . ? C19 Fe1 C21 67.3(5) . . ? C13 Fe1 C21 134.8(5) . . ? C20 Fe1 C21 39.9(5) . . ? C17 Fe1 C21 109.8(5) . . ? C15 Fe1 C21 143.2(4) . . ? C16 Fe1 C21 113.9(5) . . ? C5 N1 C6 175.1(9) . . ? C13 P1 C41 103.9(4) . . ? C13 P1 C35 102.6(4) . . ? C41 P1 C35 99.5(4) . . ? C13 P1 Ru1 118.6(3) . . ? C41 P1 Ru1 117.9(3) . . ? C35 P1 Ru1 111.7(3) . . ? C18 P2 C23 108.1(4) . . ? C18 P2 C29 98.9(4) . . ? C23 P2 C29 102.2(4) . . ? C18 P2 Ru1 116.3(3) . . ? C23 P2 Ru1 111.4(3) . . ? C29 P2 Ru1 118.4(3) . . ? C47 Ru1 C5 173.4(3) . . ? C47 Ru1 C2 86.2(4) . . ? C5 Ru1 C2 98.3(4) . . ? C47 Ru1 C1 102.9(4) . . ? C5 Ru1 C1 83.5(4) . . ? C2 Ru1 C1 36.4(3) . . ? C47 Ru1 C3 98.9(4) . . ? C5 Ru1 C3 82.3(4) . . ? C2 Ru1 C3 35.5(3) . . ? C1 Ru1 C3 64.6(4) . . ? C47 Ru1 P2 84.9(3) . . ? C5 Ru1 P2 88.5(2) . . ? C2 Ru1 P2 130.1(3) . . ? C1 Ru1 P2 161.9(3) . . ? C3 Ru1 P2 98.3(3) . . ? C47 Ru1 P1 94.3(3) . . ? C5 Ru1 P1 87.2(3) . . ? C2 Ru1 P1 124.2(3) . . ? C1 Ru1 P1 90.5(3) . . ? C3 Ru1 P1 153.8(3) . . ? P2 Ru1 P1 105.37(9) . . ? F1 Sb1 F2 89.5(4) . . ? F1 Sb1 F5 91.4(3) . . ? F2 Sb1 F5 178.8(4) . . ? F1 Sb1 F3 91.2(4) . . ? F2 Sb1 F3 91.7(4) . . ? F5 Sb1 F3 89.1(4) . . ? F1 Sb1 F6 89.6(3) . . ? F2 Sb1 F6 90.3(4) . . ? F5 Sb1 F6 88.9(4) . . ? F3 Sb1 F6 177.9(4) . . ? F1 Sb1 F4 178.6(3) . . ? F2 Sb1 F4 89.3(4) . . ? F5 Sb1 F4 89.8(4) . . ? F3 Sb1 F4 88.1(4) . . ? F6 Sb1 F4 91.1(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.737 _refine_diff_density_min -0.792 _refine_diff_density_rms 0.144 #==END