# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2086 data_global # (eta6-arene)ruthenium(II) complexes containing enantiomerically # pure (beta-aminoalkyl)phosphines or a # (beta-aminoalkyl)phosphinite: synthesis, # stereochemical and kinetic studies # # by Carmela G. Arena, Stefania Calamia, Felice Faraone # Claudia Graiff and Antonio Tiripicchio # # Submitted to Dalton Transactions # #--------------------------------- # Person for contact _publ_contact_author ; Prof. Antonio Tiripicchio Dipartimento di Chimica Generale ed Inorganica , Chimica Analitica , Chimica Fisica , University of Parma, Centro di studio per la Strutturistica diffrattometrica del CNR Viale delle Scienze, I-43100 Parma, Italy ; _publ_contact_author_email TIRI@IPRUNIV.CCE.UNIPR.IT #-------------------------------------- # Publication details loop_ _publ_author_name 'Arena, G. A.' 'Calamia, S.' 'Faraone, F.' 'Graiff, C.' 'Tiripicchio, A.' _journal_name_full 'Journal of the Chemical Society, Dalton Transactions' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '2000' #-------------------------------------- #Data for compound (5a) data_fara6h _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H40 Cl2 N P Ru' _chemical_formula_weight 653.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic ' _symmetry_space_group_name_H-M 'P212121' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 17.149(5) _cell_length_b 17.903(5) _cell_length_c 10.066(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3090.4(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red-orange' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.755 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.7519 _exptl_absorpt_correction_T_max 1 _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 'Philips PW 1100' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4153 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0732 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 28.01 _reflns_number_total 4153 _reflns_number_gt 3167 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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 _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.09(4) _refine_ls_number_reflns 4153 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0603 _refine_ls_wR_factor_gt 0.0551 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.868 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.646053(18) 0.377667(18) 0.77900(3) 0.02110(8) Uani 1 d . . . Cl1 Cl 0.76507(6) 0.32386(7) 0.86588(12) 0.0388(3) Uani 1 d . . . Cl2 Cl 0.70800(6) 0.38187(7) 0.56255(11) 0.0353(3) Uani 1 d . . . P1 P 0.61132(6) 0.25211(6) 0.73397(12) 0.0212(2) Uani 1 d . . . N1 N 0.7347(2) 0.1232(2) 0.4594(4) 0.0390(9) Uani 1 d . . . C1 C 0.6259(2) 0.4319(2) 0.9734(4) 0.0307(11) Uani 1 d . . . C2 C 0.6614(3) 0.4850(2) 0.8878(5) 0.0334(11) Uani 1 d . . . H2 H 0.7063 0.5099 0.9146 0.044(7) Uiso 1 calc R . . C3 C 0.6288(3) 0.4998(2) 0.7635(5) 0.0395(13) Uani 1 d . . . H3 H 0.6528 0.5348 0.7087 0.044(7) Uiso 1 calc R . . C4 C 0.5609(3) 0.4635(2) 0.7182(5) 0.0365(11) Uani 1 d . . . C5 C 0.5263(2) 0.4118(2) 0.8046(5) 0.0363(12) Uani 1 d . . . H5 H 0.4815 0.3868 0.7777 0.044(7) Uiso 1 calc R . . C6 C 0.5580(3) 0.3964(2) 0.9320(5) 0.0323(11) Uani 1 d . . . H6 H 0.5332 0.3626 0.9879 0.044(7) Uiso 1 calc R . . C7 C 0.6619(3) 0.4193(3) 1.1103(4) 0.0420(13) Uani 1 d . . . H7 H 0.7187 0.4230 1.1007 0.10(2) Uiso 1 calc R . . C8 C 0.6357(3) 0.4817(3) 1.2038(5) 0.0605(16) Uani 1 d . . . H8A H 0.6588 0.4744 1.2897 0.106(9) Uiso 1 calc R . . H8B H 0.5799 0.4808 1.2119 0.106(9) Uiso 1 calc R . . H8C H 0.6518 0.5291 1.1687 0.106(9) Uiso 1 calc R . . C9 C 0.6435(4) 0.3417(3) 1.1679(5) 0.078(2) Uani 1 d . . . H9A H 0.6684 0.3364 1.2528 0.106(9) Uiso 1 calc R . . H9B H 0.6624 0.3038 1.1086 0.106(9) Uiso 1 calc R . . H9C H 0.5881 0.3365 1.1784 0.106(9) Uiso 1 calc R . . C10 C 0.5276(3) 0.4805(3) 0.5813(6) 0.0633(18) Uani 1 d . . . H10A H 0.4818 0.4507 0.5668 0.124(16) Uiso 1 calc R . . H10B H 0.5658 0.4691 0.5147 0.124(16) Uiso 1 calc R . . H10C H 0.5141 0.5325 0.5762 0.124(16) Uiso 1 calc R . . C11 C 0.5791(2) 0.2025(2) 0.8822(4) 0.0237(10) Uani 1 d . . . C12 C 0.5049(3) 0.2141(3) 0.9333(5) 0.0352(12) Uani 1 d . . . H12 H 0.4703 0.2446 0.8874 0.051(7) Uiso 1 calc R . . C13 C 0.4813(3) 0.1808(3) 1.0528(5) 0.0417(13) Uani 1 d . . . H13 H 0.4311 0.1887 1.0846 0.051(7) Uiso 1 calc R . . C14 C 0.5318(3) 0.1369(3) 1.1225(5) 0.0424(13) Uani 1 d . . . H14 H 0.5162 0.1152 1.2020 0.051(7) Uiso 1 calc R . . C15 C 0.6055(3) 0.1251(3) 1.0750(4) 0.0422(12) Uani 1 d . . . H15 H 0.6399 0.0952 1.1228 0.051(7) Uiso 1 calc R . . C16 C 0.6295(3) 0.1571(2) 0.9562(4) 0.0335(12) Uani 1 d . . . H16 H 0.6798 0.1483 0.9253 0.051(7) Uiso 1 calc R . . C17 C 0.5308(2) 0.2389(2) 0.6159(4) 0.0245(10) Uani 1 d . . . C18 C 0.5311(3) 0.2816(2) 0.5009(5) 0.0333(11) Uani 1 d . . . H18 H 0.5679 0.3193 0.4910 0.035(6) Uiso 1 calc R . . C19 C 0.4773(3) 0.2691(3) 0.4008(5) 0.0436(13) Uani 1 d . . . H19 H 0.4785 0.2981 0.3241 0.035(6) Uiso 1 calc R . . C20 C 0.4219(3) 0.2137(3) 0.4146(5) 0.0439(13) Uani 1 d . . . H20 H 0.3859 0.2051 0.3471 0.035(6) Uiso 1 calc R . . C21 C 0.4201(3) 0.1717(3) 0.5274(5) 0.0432(13) Uani 1 d . . . H21 H 0.3821 0.1350 0.5376 0.035(6) Uiso 1 calc R . . C22 C 0.4748(3) 0.1834(3) 0.6273(5) 0.0375(12) Uani 1 d . . . H22 H 0.4738 0.1536 0.7029 0.035(6) Uiso 1 calc R . . C23 C 0.6916(2) 0.1990(2) 0.6592(4) 0.0284(11) Uani 1 d . . . H23A H 0.7252 0.2345 0.6143 0.036(9) Uiso 1 calc R . . H23B H 0.7217 0.1775 0.7312 0.036(9) Uiso 1 calc R . . C24 C 0.6734(2) 0.1353(2) 0.5595(4) 0.0298(11) Uani 1 d . . . H24 H 0.6263 0.1501 0.5111 0.033(14) Uiso 1 calc R . . C25 C 0.8089(3) 0.0990(3) 0.5137(6) 0.075(2) Uani 1 d . . . H25A H 0.8006 0.0576 0.5726 0.093(9) Uiso 1 calc R . . H25B H 0.8324 0.1395 0.5617 0.093(9) Uiso 1 calc R . . H25C H 0.8427 0.0839 0.4426 0.093(9) Uiso 1 calc R . . C26 C 0.7434(4) 0.1869(3) 0.3702(5) 0.0692(19) Uani 1 d . . . H26A H 0.6931 0.2011 0.3365 0.093(9) Uiso 1 calc R . . H26B H 0.7768 0.1735 0.2975 0.093(9) Uiso 1 calc R . . H26C H 0.7659 0.2281 0.4178 0.093(9) Uiso 1 calc R . . C27 C 0.6539(3) 0.0635(2) 0.6332(5) 0.0376(11) Uani 1 d . . . H27A H 0.6060 0.0711 0.6825 0.076(13) Uiso 1 calc R . . H27B H 0.6950 0.0537 0.6971 0.076(13) Uiso 1 calc R . . C28 C 0.6444(3) -0.0047(2) 0.5460(4) 0.0310(10) Uani 1 d . . . C29 C 0.6057(3) -0.0029(3) 0.4264(5) 0.0435(13) Uani 1 d . . . H29 H 0.5842 0.0419 0.3975 0.048(7) Uiso 1 calc R . . C30 C 0.5981(3) -0.0655(3) 0.3482(5) 0.0496(14) Uani 1 d . . . H30 H 0.5719 -0.0628 0.2674 0.048(7) Uiso 1 calc R . . C31 C 0.6294(3) -0.1325(3) 0.3906(5) 0.0504(15) Uani 1 d . . . H31 H 0.6263 -0.1747 0.3370 0.048(7) Uiso 1 calc R . . C32 C 0.6652(3) -0.1363(3) 0.5129(5) 0.0453(14) Uani 1 d . . . H32 H 0.6835 -0.1818 0.5448 0.048(7) Uiso 1 calc R . . C33 C 0.6738(3) -0.0722(3) 0.5880(5) 0.0384(12) Uani 1 d . . . H33 H 0.7001 -0.0748 0.6687 0.048(7) Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02074(14) 0.02112(14) 0.02144(15) -0.00165(17) 0.00168(16) -0.00103(16) Cl1 0.0281(6) 0.0436(7) 0.0448(8) -0.0083(6) -0.0082(6) 0.0072(5) Cl2 0.0394(6) 0.0362(6) 0.0303(6) 0.0002(6) 0.0120(5) -0.0060(6) P1 0.0216(5) 0.0214(5) 0.0207(6) -0.0009(5) -0.0005(5) -0.0002(4) N1 0.046(2) 0.035(2) 0.036(2) -0.008(2) 0.0099(19) 0.003(2) C1 0.035(3) 0.031(2) 0.026(2) -0.008(2) 0.004(2) 0.000(2) C2 0.033(3) 0.028(2) 0.040(3) -0.012(2) 0.003(2) -0.002(2) C3 0.050(3) 0.016(2) 0.053(4) 0.000(2) 0.007(3) 0.003(2) C4 0.039(3) 0.029(2) 0.041(3) -0.002(3) -0.001(3) 0.015(2) C5 0.022(2) 0.039(3) 0.048(3) -0.014(3) -0.002(2) 0.009(2) C6 0.034(3) 0.031(3) 0.033(3) -0.009(2) 0.012(2) -0.005(2) C7 0.049(4) 0.050(3) 0.027(3) -0.012(2) 0.003(2) -0.001(3) C8 0.073(4) 0.068(4) 0.040(3) -0.025(3) 0.000(3) -0.010(3) C9 0.137(6) 0.060(4) 0.038(3) 0.010(3) -0.012(4) -0.016(5) C10 0.076(4) 0.062(4) 0.052(4) 0.005(3) -0.025(4) 0.029(3) C11 0.028(2) 0.022(2) 0.022(2) 0.0001(19) 0.003(2) -0.0053(19) C12 0.037(3) 0.034(3) 0.034(3) 0.001(2) 0.000(2) 0.005(2) C13 0.045(3) 0.040(3) 0.040(3) 0.002(3) 0.015(3) -0.003(3) C14 0.062(3) 0.043(3) 0.023(3) 0.007(2) 0.008(3) -0.005(3) C15 0.058(3) 0.039(3) 0.030(3) 0.011(3) -0.009(2) 0.000(3) C16 0.034(3) 0.036(3) 0.031(3) 0.003(2) -0.005(2) -0.001(2) C17 0.030(2) 0.024(2) 0.020(2) -0.004(2) -0.001(2) 0.001(2) C18 0.031(3) 0.037(3) 0.032(3) 0.001(2) -0.003(2) -0.006(2) C19 0.046(3) 0.054(3) 0.031(3) 0.010(3) -0.009(3) -0.004(3) C20 0.040(3) 0.058(3) 0.034(3) -0.001(3) -0.017(3) -0.005(3) C21 0.041(3) 0.044(3) 0.045(3) 0.005(3) -0.013(3) -0.019(3) C22 0.043(3) 0.034(3) 0.036(3) 0.012(2) -0.010(2) -0.008(2) C23 0.028(2) 0.027(2) 0.029(3) -0.009(2) 0.001(2) -0.001(2) C24 0.031(2) 0.027(3) 0.031(2) -0.005(2) 0.002(2) 0.002(2) C25 0.045(4) 0.079(5) 0.101(5) -0.024(4) 0.004(4) 0.009(3) C26 0.101(5) 0.054(4) 0.053(4) -0.005(3) 0.028(4) -0.012(4) C27 0.055(3) 0.025(2) 0.032(3) -0.004(2) 0.001(3) -0.002(3) C28 0.037(2) 0.022(2) 0.034(3) -0.004(2) 0.005(3) 0.000(2) C29 0.055(3) 0.031(3) 0.045(3) -0.003(3) -0.006(3) -0.003(3) C30 0.055(3) 0.053(3) 0.040(3) -0.012(3) -0.005(3) -0.005(3) C31 0.043(3) 0.046(3) 0.062(4) -0.024(3) 0.011(3) -0.010(3) C32 0.042(3) 0.027(3) 0.067(4) -0.007(3) 0.009(3) 0.003(2) C33 0.040(3) 0.035(3) 0.041(3) -0.007(2) 0.001(2) -0.003(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 C5 2.157(4) . ? Ru1 C6 2.183(4) . ? Ru1 C4 2.206(4) . ? Ru1 C1 2.211(4) . ? Ru1 C3 2.212(4) . ? Ru1 C2 2.227(4) . ? Ru1 P1 2.3693(12) . ? Ru1 Cl1 2.4204(13) . ? Ru1 Cl2 2.4251(13) . ? P1 C11 1.823(4) . ? P1 C17 1.837(4) . ? P1 C23 1.834(4) . ? N1 C25 1.450(6) . ? N1 C26 1.461(6) . ? N1 C24 1.473(5) . ? C1 C2 1.420(6) . ? C1 C6 1.390(6) . ? C1 C7 1.527(6) . ? C2 C3 1.396(6) . ? C3 C4 1.410(6) . ? C4 C5 1.402(6) . ? C4 C10 1.523(7) . ? C5 C6 1.419(6) . ? C7 C8 1.529(6) . ? C7 C9 1.538(6) . ? C11 C12 1.388(6) . ? C11 C16 1.400(5) . ? C12 C13 1.402(6) . ? C13 C14 1.364(6) . ? C14 C15 1.367(6) . ? C15 C16 1.389(6) . ? C17 C18 1.387(6) . ? C17 C22 1.386(6) . ? C18 C19 1.384(6) . ? C19 C20 1.382(6) . ? C20 C21 1.362(6) . ? C21 C22 1.393(6) . ? C23 C24 1.551(5) . ? C24 C27 1.522(5) . ? C27 C28 1.514(5) . ? C28 C29 1.374(6) . ? C28 C33 1.376(6) . ? C29 C30 1.376(6) . ? C30 C31 1.381(7) . ? C31 C32 1.377(7) . ? C32 C33 1.382(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Ru1 C6 38.17(16) . . ? C5 Ru1 C4 37.45(16) . . ? C6 Ru1 C4 68.31(18) . . ? C5 Ru1 C1 67.76(17) . . ? C6 Ru1 C1 36.89(15) . . ? C4 Ru1 C1 80.58(18) . . ? C5 Ru1 C3 66.53(17) . . ? C6 Ru1 C3 78.78(17) . . ? C4 Ru1 C3 37.22(16) . . ? C1 Ru1 C3 66.90(18) . . ? C5 Ru1 C2 79.03(17) . . ? C6 Ru1 C2 66.55(16) . . ? C4 Ru1 C2 67.29(17) . . ? C1 Ru1 C2 37.31(15) . . ? C3 Ru1 C2 36.65(16) . . ? C5 Ru1 P1 92.98(12) . . ? C6 Ru1 P1 96.14(12) . . ? C4 Ru1 P1 116.18(13) . . ? C1 Ru1 P1 123.12(12) . . ? C3 Ru1 P1 152.98(13) . . ? C2 Ru1 P1 160.43(12) . . ? C5 Ru1 Cl1 150.69(14) . . ? C6 Ru1 Cl1 112.94(13) . . ? C4 Ru1 Cl1 159.32(13) . . ? C1 Ru1 Cl1 89.24(12) . . ? C3 Ru1 Cl1 122.11(13) . . ? C2 Ru1 Cl1 93.79(12) . . ? P1 Ru1 Cl1 84.46(4) . . ? C5 Ru1 Cl2 121.02(14) . . ? C6 Ru1 Cl2 158.76(12) . . ? C4 Ru1 Cl2 91.10(14) . . ? C1 Ru1 Cl2 148.19(12) . . ? C3 Ru1 Cl2 87.96(14) . . ? C2 Ru1 Cl2 111.31(12) . . ? P1 Ru1 Cl2 88.15(4) . . ? Cl1 Ru1 Cl2 88.14(5) . . ? C11 P1 C17 103.83(19) . . ? C11 P1 C23 108.1(2) . . ? C17 P1 C23 103.40(19) . . ? C11 P1 Ru1 112.48(14) . . ? C17 P1 Ru1 115.78(14) . . ? C23 P1 Ru1 112.42(14) . . ? C25 N1 C26 112.1(4) . . ? C25 N1 C24 114.4(4) . . ? C26 N1 C24 112.2(4) . . ? C2 C1 C6 118.9(4) . . ? C2 C1 C7 118.2(4) . . ? C6 C1 C7 122.8(4) . . ? C2 C1 Ru1 71.9(2) . . ? C6 C1 Ru1 70.5(2) . . ? C7 C1 Ru1 132.1(3) . . ? C1 C2 C3 120.0(4) . . ? C1 C2 Ru1 70.8(2) . . ? C3 C2 Ru1 71.1(2) . . ? C4 C3 C2 122.2(4) . . ? C4 C3 Ru1 71.2(2) . . ? C2 C3 Ru1 72.3(2) . . ? C3 C4 C5 117.0(5) . . ? C3 C4 C10 120.7(5) . . ? C5 C4 C10 122.4(5) . . ? C3 C4 Ru1 71.6(2) . . ? C5 C4 Ru1 69.4(2) . . ? C10 C4 Ru1 129.7(3) . . ? C4 C5 C6 121.8(4) . . ? C4 C5 Ru1 73.2(2) . . ? C6 C5 Ru1 71.9(2) . . ? C1 C6 C5 120.2(4) . . ? C1 C6 Ru1 72.7(3) . . ? C5 C6 Ru1 69.9(2) . . ? C1 C7 C8 109.2(4) . . ? C1 C7 C9 113.0(4) . . ? C8 C7 C9 111.5(4) . . ? C12 C11 C16 117.1(4) . . ? C12 C11 P1 120.5(3) . . ? C16 C11 P1 122.1(3) . . ? C13 C12 C11 121.3(5) . . ? C12 C13 C14 120.2(5) . . ? C15 C14 C13 119.8(5) . . ? C14 C15 C16 120.7(5) . . ? C15 C16 C11 121.0(4) . . ? C18 C17 C22 117.8(4) . . ? C18 C17 P1 117.8(3) . . ? C22 C17 P1 124.0(3) . . ? C17 C18 C19 121.1(4) . . ? C20 C19 C18 120.1(5) . . ? C21 C20 C19 119.7(5) . . ? C20 C21 C22 120.3(5) . . ? C21 C22 C17 121.0(4) . . ? C24 C23 P1 119.7(3) . . ? N1 C24 C27 111.4(4) . . ? N1 C24 C23 114.1(3) . . ? C27 C24 C23 110.5(4) . . ? C24 C27 C28 115.0(4) . . ? C29 C28 C33 117.9(4) . . ? C29 C28 C27 122.7(4) . . ? C33 C28 C27 119.4(4) . . ? C30 C29 C28 121.8(5) . . ? C29 C30 C31 119.6(5) . . ? C32 C31 C30 119.5(5) . . ? C31 C32 C33 119.7(5) . . ? C32 C33 C28 121.4(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.872 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.074 #===END data_f17h _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C32 H38 Cl N P Ru . B F4 ' _chemical_formula_sum 'C32 H38 B Cl F4 N P Ru' _chemical_formula_weight 690.93 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' 'Cl' 'Cl' 0.1484 0.1585 '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' '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' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P212121' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.866(4) _cell_length_b 24.897(5) _cell_length_c 11.912(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3222.6(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type 'software SMART' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AMX SMART 1000' _diffrn_measurement_method 'Software SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19073 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.01 _reflns_number_total 6908 _reflns_number_gt 6467 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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 _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(2) _refine_ls_number_reflns 6908 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F1 F 0.0997(3) 0.55518(13) 0.9902(3) 0.1138(11) Uani 1 d . . . F2 F 0.1023(4) 0.56565(19) 1.1711(3) 0.1461(15) Uani 1 d . . . F3 F 0.1332(3) 0.63569(12) 1.0629(4) 0.1229(12) Uani 1 d . . . F4 F -0.0558(2) 0.60061(14) 1.0762(3) 0.1023(9) Uani 1 d . . . B1 B 0.0662(4) 0.59010(18) 1.0735(4) 0.0582(9) Uani 1 d . . . Ru1 Ru 0.039451(19) 0.877396(8) 0.774218(17) 0.03719(7) Uani 1 d . . . P1 P 0.16150(7) 0.91233(3) 0.63219(6) 0.03981(16) Uani 1 d . . . N1 N -0.1051(2) 0.88487(10) 0.6406(2) 0.0429(5) Uani 1 d . . . Cl1 Cl 0.07968(8) 0.79136(3) 0.69465(7) 0.05382(19) Uani 1 d . . . C1 C 0.0332(3) 0.83323(13) 0.9436(2) 0.0507(7) Uani 1 d . . . C2 C 0.1476(3) 0.86032(14) 0.9250(2) 0.0493(7) Uani 1 d . . . H2 H 0.2208 0.8410 0.9267 0.048(4) Uiso 1 calc R . . C3 C 0.1504(3) 0.91563(14) 0.9045(3) 0.0488(7) Uani 1 d . . . H3 H 0.2258 0.9326 0.8946 0.048(4) Uiso 1 calc R . . C4 C 0.0401(4) 0.94647(12) 0.8985(2) 0.0503(7) Uani 1 d . . . C5 C -0.0704(3) 0.91846(15) 0.9067(3) 0.0544(8) Uani 1 d . . . H5 H -0.1436 0.9371 0.8959 0.048(4) Uiso 1 calc R . . C6 C -0.0764(3) 0.86240(14) 0.9312(3) 0.0517(8) Uani 1 d . . . H6 H -0.1521 0.8454 0.9388 0.048(4) Uiso 1 calc R . . C7 C 0.0345(5) 0.77417(14) 0.9742(3) 0.0667(9) Uani 1 d . . . H7 H 0.1021 0.7574 0.9326 0.056(10) Uiso 1 calc R . . C8 C 0.0661(6) 0.77034(18) 1.1004(3) 0.0955(17) Uani 1 d . . . H8A H 0.1425 0.7885 1.1145 0.124(9) Uiso 1 calc R . . H8B H 0.0736 0.7333 1.1215 0.124(9) Uiso 1 calc R . . H8C H 0.0019 0.7869 1.1436 0.124(9) Uiso 1 calc R . . C9 C -0.0829(6) 0.7445(2) 0.9432(5) 0.1081(19) Uani 1 d . . . H9A H -0.0753 0.7074 0.9639 0.124(9) Uiso 1 calc R . . H9B H -0.0963 0.7472 0.8637 0.124(9) Uiso 1 calc R . . H9C H -0.1512 0.7602 0.9823 0.124(9) Uiso 1 calc R . . C10 C 0.0454(5) 1.00661(14) 0.8884(3) 0.0766(12) Uani 1 d . . . H10A H 0.1297 1.0179 0.8833 0.135(12) Uiso 1 calc R . . H10B H 0.0080 1.0227 0.9532 0.135(12) Uiso 1 calc R . . H10C H 0.0020 1.0177 0.8221 0.135(12) Uiso 1 calc R . . C11 C 0.2346(3) 0.97764(12) 0.6526(2) 0.0465(7) Uani 1 d . . . C12 C 0.3541(3) 0.98054(16) 0.6928(3) 0.0612(9) Uani 1 d . . . H12 H 0.3979 0.9491 0.7060 0.084(6) Uiso 1 calc R . . C13 C 0.4088(4) 1.02949(19) 0.7134(3) 0.0789(12) Uani 1 d . . . H13 H 0.4891 1.0308 0.7403 0.084(6) Uiso 1 calc R . . C14 C 0.3461(5) 1.07596(18) 0.6947(3) 0.0784(13) Uani 1 d . . . H14 H 0.3838 1.1088 0.7088 0.084(6) Uiso 1 calc R . . C15 C 0.2272(5) 1.07454(16) 0.6550(3) 0.0737(12) Uani 1 d . . . H15 H 0.1844 1.1063 0.6424 0.084(6) Uiso 1 calc R . . C16 C 0.1713(4) 1.02504(13) 0.6339(3) 0.0577(8) Uani 1 d . . . H16 H 0.0910 1.0239 0.6072 0.084(6) Uiso 1 calc R . . C17 C 0.2883(3) 0.87042(12) 0.5834(2) 0.0451(6) Uani 1 d . . . C18 C 0.3603(3) 0.84342(17) 0.6600(3) 0.0618(9) Uani 1 d . . . H18 H 0.3400 0.8448 0.7358 0.102(7) Uiso 1 calc R . . C19 C 0.4630(4) 0.81394(18) 0.6261(3) 0.0717(10) Uani 1 d . . . H19 H 0.5128 0.7973 0.6793 0.102(7) Uiso 1 calc R . . C20 C 0.4899(4) 0.80969(17) 0.5153(4) 0.0698(10) Uani 1 d . . . H20 H 0.5569 0.7891 0.4926 0.102(7) Uiso 1 calc R . . C21 C 0.4210(4) 0.83481(19) 0.4384(4) 0.0813(12) Uani 1 d . . . H21 H 0.4412 0.8317 0.3628 0.102(7) Uiso 1 calc R . . C22 C 0.3177(4) 0.86618(16) 0.4702(3) 0.0643(9) Uani 1 d . . . H22 H 0.2705 0.8836 0.4162 0.102(7) Uiso 1 calc R . . C23 C 0.0556(3) 0.92019(13) 0.5142(2) 0.0476(7) Uani 1 d . . . H23A H 0.0211 0.9561 0.5141 0.082(9) Uiso 1 calc R . . H23B H 0.0990 0.9148 0.4439 0.082(9) Uiso 1 calc R . . C24 C -0.0466(3) 0.87881(11) 0.5263(2) 0.0406(5) Uani 1 d . . . H24 H -0.0058 0.8437 0.5267 0.035(7) Uiso 1 calc R . . C25 C -0.1716(3) 0.93758(14) 0.6500(3) 0.0551(8) Uani 1 d . . . H25A H -0.1143 0.9665 0.6390 0.068(4) Uiso 1 calc R . . H25B H -0.2079 0.9406 0.7232 0.068(4) Uiso 1 calc R . . H25C H -0.2349 0.9394 0.5939 0.068(4) Uiso 1 calc R . . C26 C -0.1983(3) 0.84163(16) 0.6571(3) 0.0597(9) Uani 1 d . . . H26A H -0.1590 0.8072 0.6517 0.068(4) Uiso 1 calc R . . H26B H -0.2607 0.8445 0.6003 0.068(4) Uiso 1 calc R . . H26C H -0.2354 0.8454 0.7298 0.068(4) Uiso 1 calc R . . C27 C -0.1327(3) 0.87837(12) 0.4257(2) 0.0430(6) Uani 1 d . . . C28 C -0.1669(4) 0.82944(13) 0.3804(3) 0.0595(9) Uani 1 d . . . H28 H -0.1420 0.7979 0.4155 0.072(5) Uiso 1 calc R . . C29 C -0.2375(4) 0.82656(18) 0.2843(3) 0.0775(12) Uani 1 d . . . H29 H -0.2591 0.7932 0.2549 0.072(5) Uiso 1 calc R . . C30 C -0.2757(4) 0.87241(18) 0.2321(3) 0.0769(11) Uani 1 d . . . H30 H -0.3227 0.8705 0.1669 0.072(5) Uiso 1 calc R . . C31 C -0.2442(3) 0.92161(16) 0.2766(3) 0.0657(9) Uani 1 d . . . H31 H -0.2706 0.9528 0.2411 0.072(5) Uiso 1 calc R . . C32 C -0.1741(3) 0.92529(13) 0.3731(3) 0.0530(7) Uani 1 d . . . H32 H -0.1546 0.9587 0.4029 0.072(5) Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.116(3) 0.105(2) 0.121(2) -0.0374(18) 0.024(2) -0.0081(19) F2 0.106(3) 0.224(4) 0.109(2) 0.048(3) -0.022(2) 0.006(3) F3 0.084(2) 0.0831(19) 0.202(4) -0.017(2) 0.016(2) -0.0232(15) F4 0.0509(15) 0.151(3) 0.1054(19) -0.0078(18) -0.0076(14) -0.0011(15) B1 0.040(2) 0.074(2) 0.060(2) -0.0039(18) 0.0009(16) -0.0104(17) Ru1 0.03254(11) 0.04167(11) 0.03737(10) 0.00132(8) -0.00037(8) 0.00039(9) P1 0.0316(3) 0.0514(4) 0.0364(3) 0.0016(3) -0.0022(3) -0.0030(3) N1 0.0339(12) 0.0505(13) 0.0442(11) 0.0039(10) 0.0016(10) -0.0019(11) Cl1 0.0618(5) 0.0432(3) 0.0564(4) -0.0018(3) -0.0038(3) 0.0072(3) C1 0.0523(18) 0.0574(17) 0.0423(14) 0.0074(12) 0.0037(14) 0.0023(16) C2 0.0434(17) 0.066(2) 0.0386(14) 0.0078(13) -0.0038(13) 0.0041(14) C3 0.0476(18) 0.0617(19) 0.0369(14) 0.0013(13) -0.0057(13) -0.0091(15) C4 0.063(2) 0.0519(16) 0.0358(13) -0.0038(11) -0.0036(15) -0.0025(16) C5 0.0503(19) 0.070(2) 0.0426(15) -0.0058(14) 0.0018(14) 0.0172(15) C6 0.0373(15) 0.070(2) 0.0482(16) 0.0046(14) 0.0062(13) -0.0034(13) C7 0.085(3) 0.0544(18) 0.0604(18) 0.0155(14) 0.010(2) 0.001(2) C8 0.152(5) 0.072(2) 0.062(2) 0.0232(18) 0.017(3) 0.019(3) C9 0.121(5) 0.078(3) 0.125(4) 0.020(3) 0.010(4) -0.038(3) C10 0.120(4) 0.0511(18) 0.0583(19) -0.0068(14) -0.008(2) 0.001(2) C11 0.0419(16) 0.0592(17) 0.0382(13) 0.0026(12) 0.0011(12) -0.0094(13) C12 0.053(2) 0.079(2) 0.0516(17) -0.0056(16) -0.0081(15) -0.0154(17) C13 0.071(3) 0.100(3) 0.066(2) -0.008(2) -0.014(2) -0.034(2) C14 0.111(4) 0.074(2) 0.0508(19) 0.0006(17) -0.002(2) -0.042(3) C15 0.109(4) 0.058(2) 0.055(2) 0.0069(16) -0.002(2) -0.016(2) C16 0.066(2) 0.0560(18) 0.0507(16) 0.0077(14) -0.0024(16) -0.0078(16) C17 0.0360(14) 0.0526(17) 0.0468(13) -0.0048(13) 0.0012(12) -0.0040(13) C18 0.0395(18) 0.094(3) 0.0520(18) 0.0013(17) 0.0051(14) 0.0140(17) C19 0.0454(19) 0.097(3) 0.073(2) -0.002(2) 0.005(2) 0.016(2) C20 0.048(2) 0.074(2) 0.087(2) -0.018(2) 0.0069(19) 0.0094(17) C21 0.075(3) 0.103(3) 0.066(2) -0.023(2) 0.021(2) 0.010(2) C22 0.062(2) 0.081(2) 0.0500(16) -0.0061(16) 0.0066(16) 0.0110(19) C23 0.0357(16) 0.0665(18) 0.0405(13) 0.0047(12) -0.0069(12) -0.0058(14) C24 0.0365(14) 0.0421(13) 0.0433(12) 0.0000(11) -0.0048(11) -0.0001(15) C25 0.0476(18) 0.068(2) 0.0499(16) -0.0017(14) -0.0015(15) 0.0188(15) C26 0.0462(19) 0.077(2) 0.0558(19) 0.0099(16) -0.0101(15) -0.0196(16) C27 0.0401(14) 0.0467(14) 0.0424(13) 0.0034(12) -0.0061(11) -0.0033(13) C28 0.070(2) 0.0528(18) 0.0555(18) -0.0008(14) -0.0104(18) -0.0135(17) C29 0.089(3) 0.084(3) 0.059(2) -0.0009(19) -0.020(2) -0.039(2) C30 0.064(2) 0.111(3) 0.0556(17) 0.012(2) -0.0230(18) -0.026(2) C31 0.055(2) 0.081(2) 0.0613(19) 0.0188(19) -0.0160(19) 0.0028(17) C32 0.0469(18) 0.0518(17) 0.0603(18) 0.0066(14) -0.0118(15) -0.0007(14) _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 F1 B1 1.369(5) . ? F2 B1 1.369(6) . ? F3 B1 1.355(5) . ? F4 B1 1.351(5) . ? Ru1 C3 2.183(3) . ? Ru1 C2 2.189(3) . ? Ru1 C5 2.228(3) . ? Ru1 N1 2.243(2) . ? Ru1 C4 2.269(3) . ? Ru1 C6 2.284(3) . ? Ru1 C1 2.298(3) . ? Ru1 P1 2.3189(9) . ? Ru1 Cl1 2.3829(8) . ? P1 C11 1.826(3) . ? P1 C17 1.823(3) . ? P1 C23 1.828(3) . ? N1 C26 1.491(4) . ? N1 C25 1.502(4) . ? N1 C24 1.511(3) . ? C1 C6 1.402(5) . ? C1 C2 1.432(5) . ? C1 C7 1.515(5) . ? C2 C3 1.399(5) . ? C3 C4 1.425(5) . ? C4 C5 1.392(5) . ? C4 C10 1.503(5) . ? C5 C6 1.427(5) . ? C7 C9 1.519(7) . ? C7 C8 1.545(6) . ? C11 C16 1.384(5) . ? C11 C12 1.386(5) . ? C12 C13 1.378(5) . ? C13 C14 1.361(7) . ? C14 C15 1.376(7) . ? C15 C16 1.397(5) . ? C17 C18 1.377(5) . ? C17 C22 1.390(4) . ? C18 C19 1.396(5) . ? C19 C20 1.356(6) . ? C20 C21 1.339(6) . ? C21 C22 1.419(5) . ? C23 C24 1.521(4) . ? C24 C27 1.520(4) . ? C27 C32 1.400(4) . ? C27 C28 1.383(4) . ? C28 C29 1.381(5) . ? C29 C30 1.365(6) . ? C30 C31 1.378(6) . ? C31 C32 1.382(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 B1 F4 110.3(4) . . ? F2 B1 F3 107.3(4) . . ? F4 B1 F3 111.6(4) . . ? F2 B1 F1 104.9(4) . . ? F4 B1 F1 113.7(4) . . ? F3 B1 F1 108.8(4) . . ? C3 Ru1 C2 37.32(13) . . ? C3 Ru1 C5 65.92(12) . . ? C2 Ru1 C5 78.19(13) . . ? C3 Ru1 N1 148.69(11) . . ? C2 Ru1 N1 166.97(10) . . ? C5 Ru1 N1 95.12(11) . . ? C3 Ru1 C4 37.27(13) . . ? C2 Ru1 C4 67.05(12) . . ? C5 Ru1 C4 36.05(13) . . ? N1 Ru1 C4 113.70(11) . . ? C3 Ru1 C6 78.09(13) . . ? C2 Ru1 C6 65.94(12) . . ? C5 Ru1 C6 36.85(14) . . ? N1 Ru1 C6 102.02(11) . . ? C4 Ru1 C6 65.89(12) . . ? C3 Ru1 C1 66.49(12) . . ? C2 Ru1 C1 37.12(13) . . ? C5 Ru1 C1 65.27(13) . . ? N1 Ru1 C1 129.88(11) . . ? C4 Ru1 C1 77.88(11) . . ? C6 Ru1 C1 35.63(12) . . ? C3 Ru1 P1 92.26(9) . . ? C2 Ru1 P1 111.39(9) . . ? C5 Ru1 P1 130.65(10) . . ? N1 Ru1 P1 81.48(7) . . ? C4 Ru1 P1 100.96(9) . . ? C6 Ru1 P1 166.77(9) . . ? C1 Ru1 P1 146.80(10) . . ? C3 Ru1 Cl1 124.99(10) . . ? C2 Ru1 Cl1 93.06(9) . . ? C5 Ru1 Cl1 142.44(10) . . ? N1 Ru1 Cl1 85.46(7) . . ? C4 Ru1 Cl1 160.09(8) . . ? C6 Ru1 Cl1 106.24(9) . . ? C1 Ru1 Cl1 85.66(8) . . ? P1 Ru1 Cl1 86.68(3) . . ? C11 P1 C17 102.90(15) . . ? C11 P1 C23 106.32(14) . . ? C17 P1 C23 106.97(14) . . ? C11 P1 Ru1 119.06(10) . . ? C17 P1 Ru1 116.75(10) . . ? C23 P1 Ru1 103.97(10) . . ? C26 N1 C25 107.1(3) . . ? C26 N1 C24 109.4(2) . . ? C25 N1 C24 110.9(2) . . ? C26 N1 Ru1 108.83(18) . . ? C25 N1 Ru1 110.87(19) . . ? C24 N1 Ru1 109.66(16) . . ? C6 C1 C2 118.5(3) . . ? C6 C1 C7 122.4(3) . . ? C2 C1 C7 119.1(3) . . ? C6 C1 Ru1 71.64(17) . . ? C2 C1 Ru1 67.27(16) . . ? C7 C1 Ru1 132.5(2) . . ? C3 C2 C1 120.6(3) . . ? C3 C2 Ru1 71.14(19) . . ? C1 C2 Ru1 75.61(18) . . ? C2 C3 C4 121.4(3) . . ? C2 C3 Ru1 71.54(19) . . ? C4 C3 Ru1 74.64(18) . . ? C5 C4 C3 116.9(3) . . ? C5 C4 C10 122.6(4) . . ? C3 C4 C10 120.5(4) . . ? C5 C4 Ru1 70.35(17) . . ? C3 C4 Ru1 68.09(17) . . ? C10 C4 Ru1 134.6(2) . . ? C4 C5 C6 122.9(3) . . ? C4 C5 Ru1 73.60(18) . . ? C6 C5 Ru1 73.73(19) . . ? C1 C6 C5 119.3(3) . . ? C1 C6 Ru1 72.73(18) . . ? C5 C6 Ru1 69.42(18) . . ? C9 C7 C1 113.9(4) . . ? C9 C7 C8 113.2(4) . . ? C1 C7 C8 107.2(3) . . ? C16 C11 C12 118.5(3) . . ? C16 C11 P1 121.4(3) . . ? C12 C11 P1 120.0(3) . . ? C11 C12 C13 120.8(4) . . ? C14 C13 C12 120.4(4) . . ? C13 C14 C15 120.3(4) . . ? C14 C15 C16 119.5(4) . . ? C11 C16 C15 120.5(4) . . ? C18 C17 C22 118.4(3) . . ? C18 C17 P1 119.8(2) . . ? C22 C17 P1 121.8(3) . . ? C17 C18 C19 121.3(3) . . ? C20 C19 C18 119.7(4) . . ? C21 C20 C19 120.6(4) . . ? C20 C21 C22 121.1(4) . . ? C17 C22 C21 118.9(4) . . ? C24 C23 P1 108.29(19) . . ? N1 C24 C27 116.9(2) . . ? N1 C24 C23 109.0(2) . . ? C27 C24 C23 112.3(2) . . ? C32 C27 C28 118.3(3) . . ? C32 C27 C24 123.0(3) . . ? C28 C27 C24 118.6(3) . . ? C29 C28 C27 121.2(3) . . ? C28 C29 C30 120.2(3) . . ? C31 C30 C29 119.5(3) . . ? C30 C31 C32 121.1(3) . . ? C27 C32 C31 119.6(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.373 _refine_diff_density_min -0.928 _refine_diff_density_rms 0.131