Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemsitry 2003 data_global _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name 'Dorota Duraczynska' 'John H. Nelson' _publ_contact_author_name 'Prof John H Nelson' _publ_contact_author_address ; Department of Chemistry /216 University of Nevada-Reno Reno Nevada 89557-0020 UNITED STATES OF AMERICA ; _publ_contact_author_email JHNELSON@UNR.EDU _publ_section_title ; Diphenylvinylphosphine (DPVP) Complexes Containing the (n5-MeC5H4)Ru(II) Moiety: Synthesis, Characterization and Reactions ; data_jhn429a _database_code_CSD 195526 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 F6 N P3 Ru' _chemical_formula_weight 790.64 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' Ru Ru -1.2594 0.8363 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.5787(10) _cell_length_b 13.166(4) _cell_length_c 20.392(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.630(8) _cell_angle_gamma 90.00 _cell_volume 3613.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 4.82 _cell_measurement_theta_max 12.47 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max .42 _exptl_crystal_size_mid .42 _exptl_crystal_size_min .42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.624 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8868 _exptl_absorpt_correction_T_max 0.9676 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7919 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6367 _reflns_number_gt 4255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0668P)^2^+2.3898P] 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 6367 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.91628(3) 1.38215(4) 0.73723(2) 0.04259(16) Uani 1 1 d . . . P1 P 1.02363(10) 1.24496(11) 0.74081(7) 0.0412(3) Uani 1 1 d . . . P2 P 0.99473(12) 1.46447(12) 0.83004(8) 0.0483(4) Uani 1 1 d . . . N1 N 1.0036(3) 1.4539(4) 0.6776(2) 0.0518(12) Uani 1 1 d . . . C1 C 0.7804(5) 1.3510(7) 0.6642(4) 0.072(2) Uani 1 1 d . . . C2 C 0.7834(4) 1.2858(6) 0.7191(4) 0.075(2) Uani 1 1 d . . . H2A H 0.7832 1.2114 0.7174 0.089 Uiso 1 1 calc R . . C3 C 0.7789(4) 1.3451(6) 0.7764(4) 0.0660(19) Uani 1 1 d . . . H3A H 0.7735 1.3192 0.8209 0.079 Uiso 1 1 calc R . . C4 C 0.7730(4) 1.4471(5) 0.7568(4) 0.0650(18) Uani 1 1 d . . . H4A H 0.7645 1.5053 0.7855 0.078 Uiso 1 1 calc R . . C5 C 0.7752(4) 1.4508(6) 0.6895(4) 0.0677(19) Uani 1 1 d . . . H5A H 0.7702 1.5130 0.6628 0.081 Uiso 1 1 calc R . . C6 C 0.7715(7) 1.3224(10) 0.5924(5) 0.154(5) Uani 1 1 d . . . H6A H 0.7027 1.3139 0.5752 0.232 Uiso 1 1 calc R . . H6B H 0.8064 1.2599 0.5879 0.232 Uiso 1 1 calc R . . H6C H 0.7999 1.3750 0.5683 0.232 Uiso 1 1 calc R . . C7 C 0.9327(5) 1.4385(6) 0.9016(3) 0.0656(18) Uani 1 1 d . . . H7A H 0.9433 1.3747 0.9208 0.079 Uiso 1 1 calc R . . C8 C 0.8747(6) 1.4999(6) 0.9289(4) 0.086(2) Uani 1 1 d . . . H8A H 0.8617 1.5646 0.9115 0.103 Uiso 1 1 calc R . . H8B H 0.8463 1.4790 0.9657 0.103 Uiso 1 1 calc R . . C9 C 0.9952(5) 1.6038(4) 0.8255(3) 0.0566(16) Uani 1 1 d . . . C10 C 1.0374(6) 1.6615(5) 0.8787(4) 0.079(2) Uani 1 1 d . . . H10A H 1.0645 1.6292 0.9174 0.095 Uiso 1 1 calc R . . C11 C 1.0400(6) 1.7666(6) 0.8752(5) 0.086(2) Uani 1 1 d . . . H11A H 1.0680 1.8048 0.9113 0.104 Uiso 1 1 calc R . . C12 C 0.9998(6) 1.8140(6) 0.8166(5) 0.091(3) Uani 1 1 d . . . H12A H 0.9998 1.8845 0.8140 0.109 Uiso 1 1 calc R . . C13 C 0.9608(5) 1.7587(6) 0.7636(4) 0.081(2) Uani 1 1 d . . . H13A H 0.9360 1.7912 0.7244 0.098 Uiso 1 1 calc R . . C14 C 0.9577(5) 1.6525(5) 0.7676(4) 0.0631(17) Uani 1 1 d . . . H14A H 0.9303 1.6147 0.7312 0.076 Uiso 1 1 calc R . . C15 C 1.1263(4) 1.4377(4) 0.8590(3) 0.0469(14) Uani 1 1 d . . . C16 C 1.1991(5) 1.4881(5) 0.8306(3) 0.0641(18) Uani 1 1 d . . . H16A H 1.1812 1.5408 0.8010 0.077 Uiso 1 1 calc R . . C17 C 1.2983(5) 1.4619(6) 0.8453(4) 0.077(2) Uani 1 1 d . . . H17A H 1.3465 1.4974 0.8262 0.092 Uiso 1 1 calc R . . C18 C 1.3249(6) 1.3839(7) 0.8878(4) 0.083(2) Uani 1 1 d . . . H18A H 1.3911 1.3639 0.8963 0.100 Uiso 1 1 calc R . . C19 C 1.2543(5) 1.3349(6) 0.9181(3) 0.076(2) Uani 1 1 d . . . H19A H 1.2734 1.2839 0.9487 0.092 Uiso 1 1 calc R . . C20 C 1.1553(5) 1.3602(5) 0.9036(3) 0.0610(17) Uani 1 1 d . . . H20A H 1.1079 1.3254 0.9238 0.073 Uiso 1 1 calc R . . C21 C 1.1524(4) 1.2723(5) 0.7330(3) 0.0525(15) Uani 1 1 d . . . H21A H 1.1862 1.3099 0.7675 0.063 Uiso 1 1 calc R . . C22 C 1.2038(5) 1.2477(6) 0.6871(4) 0.076(2) Uani 1 1 d . . . H22A H 1.1750 1.2101 0.6510 0.091 Uiso 1 1 calc R . . H22B H 1.2700 1.2674 0.6899 0.091 Uiso 1 1 calc R . . C23 C 0.9843(4) 1.1556(4) 0.6734(3) 0.0446(13) Uani 1 1 d . . . C24 C 0.9444(4) 1.0610(5) 0.6834(3) 0.0534(15) Uani 1 1 d . . . H24A H 0.9402 1.0390 0.7263 0.064 Uiso 1 1 calc R . . C25 C 0.9112(5) 0.9996(5) 0.6312(3) 0.0627(17) Uani 1 1 d . . . H25A H 0.8831 0.9370 0.6388 0.075 Uiso 1 1 calc R . . C26 C 0.9191(5) 1.0296(6) 0.5675(3) 0.0666(19) Uani 1 1 d . . . H26A H 0.8975 0.9870 0.5321 0.080 Uiso 1 1 calc R . . C27 C 0.9592(5) 1.1235(6) 0.5565(3) 0.0679(18) Uani 1 1 d . . . H27A H 0.9649 1.1442 0.5136 0.081 Uiso 1 1 calc R . . C28 C 0.9906(5) 1.1857(5) 0.6084(3) 0.0571(16) Uani 1 1 d . . . H28A H 1.0165 1.2492 0.6004 0.069 Uiso 1 1 calc R . . C29 C 1.0386(4) 1.1633(4) 0.8144(3) 0.0455(13) Uani 1 1 d . . . C30 C 0.9665(5) 1.1639(5) 0.8566(3) 0.0631(18) Uani 1 1 d . . . H30A H 0.9100 1.2038 0.8468 0.076 Uiso 1 1 calc R . . C31 C 0.9789(7) 1.1054(6) 0.9130(4) 0.093(3) Uani 1 1 d . . . H31A H 0.9310 1.1066 0.9416 0.112 Uiso 1 1 calc R . . C32 C 1.0615(7) 1.0455(6) 0.9272(4) 0.088(2) Uani 1 1 d . . . H32A H 1.0701 1.0075 0.9660 0.106 Uiso 1 1 calc R . . C33 C 1.1311(5) 1.0413(5) 0.8849(4) 0.075(2) Uani 1 1 d . . . H33A H 1.1860 0.9990 0.8940 0.090 Uiso 1 1 calc R . . C34 C 1.1194(5) 1.1001(5) 0.8287(3) 0.0601(17) Uani 1 1 d . . . H34A H 1.1668 1.0972 0.7998 0.072 Uiso 1 1 calc R . . C35 C 1.0435(5) 1.4971(6) 0.6408(4) 0.0677(19) Uani 1 1 d . . . C36 C 1.0941(6) 1.5578(8) 0.5949(5) 0.117(3) Uani 1 1 d . . . H36A H 1.0540 1.5601 0.5525 0.176 Uiso 1 1 calc R . . H36B H 1.1572 1.5275 0.5904 0.176 Uiso 1 1 calc R . . H36C H 1.1042 1.6256 0.6119 0.176 Uiso 1 1 calc R . . P3 P 0.68598(16) 1.19528(16) 0.96608(9) 0.0706(5) Uani 1 1 d . . . F1 F 0.7521(8) 1.2190(9) 0.9186(5) 0.312(7) Uani 1 1 d . . . F2 F 0.7051(8) 1.2960(6) 0.9981(6) 0.264(5) Uani 1 1 d . . . F3 F 0.6136(7) 1.1697(6) 1.0131(4) 0.217(4) Uani 1 1 d . . . F4 F 0.6541(8) 1.0973(7) 0.9338(5) 0.252(5) Uani 1 1 d . . . F5 F 0.7655(6) 1.1407(7) 1.0061(5) 0.249(5) Uani 1 1 d . . . F6 F 0.5978(7) 1.2495(8) 0.9263(5) 0.253(5) Uani 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 Ru1 0.0365(2) 0.0471(3) 0.0447(3) 0.0044(2) 0.00708(17) 0.0000(2) P1 0.0395(8) 0.0454(8) 0.0395(8) 0.0037(7) 0.0081(6) -0.0023(7) P2 0.0486(9) 0.0486(9) 0.0479(9) 0.0006(7) 0.0072(7) 0.0005(7) N1 0.044(3) 0.057(3) 0.056(3) 0.013(3) 0.015(2) 0.006(3) C1 0.043(4) 0.109(6) 0.063(4) -0.018(4) 0.000(3) -0.004(4) C2 0.034(3) 0.061(4) 0.128(7) -0.008(5) 0.007(4) -0.015(3) C3 0.040(3) 0.083(5) 0.078(5) 0.014(4) 0.017(3) -0.008(3) C4 0.039(3) 0.071(5) 0.086(5) 0.004(4) 0.013(3) 0.008(3) C5 0.044(4) 0.082(5) 0.075(5) 0.020(4) -0.001(3) 0.008(4) C6 0.095(7) 0.242(13) 0.114(8) -0.080(9) -0.035(6) 0.012(8) C7 0.070(4) 0.074(5) 0.055(4) 0.003(4) 0.017(3) 0.001(4) C8 0.087(5) 0.111(7) 0.063(4) -0.007(4) 0.022(4) 0.006(5) C9 0.055(4) 0.045(4) 0.073(4) -0.005(3) 0.018(3) -0.001(3) C10 0.080(5) 0.058(4) 0.095(6) -0.016(4) -0.005(4) -0.001(4) C11 0.085(6) 0.051(5) 0.122(7) -0.028(5) 0.007(5) -0.012(4) C12 0.071(5) 0.057(5) 0.142(8) 0.002(6) 0.005(5) 0.006(4) C13 0.055(4) 0.065(5) 0.119(7) 0.012(5) -0.004(4) 0.005(4) C14 0.054(4) 0.051(4) 0.084(5) -0.003(4) 0.010(4) -0.001(3) C15 0.050(3) 0.047(3) 0.042(3) 0.001(3) -0.001(3) -0.001(3) C16 0.058(4) 0.061(4) 0.071(4) 0.011(4) 0.003(3) -0.004(3) C17 0.048(4) 0.091(6) 0.088(5) 0.007(5) -0.001(4) -0.019(4) C18 0.055(4) 0.103(6) 0.086(5) 0.001(5) -0.015(4) 0.001(5) C19 0.070(5) 0.083(5) 0.069(5) 0.014(4) -0.020(4) 0.005(4) C20 0.061(4) 0.065(4) 0.054(4) 0.001(3) -0.002(3) -0.011(3) C21 0.040(3) 0.061(4) 0.057(4) 0.004(3) 0.009(3) -0.005(3) C22 0.054(4) 0.093(6) 0.087(5) -0.002(4) 0.027(4) -0.011(4) C23 0.040(3) 0.046(3) 0.049(3) 0.000(3) 0.011(3) -0.002(3) C24 0.051(4) 0.059(4) 0.052(4) -0.002(3) 0.012(3) -0.008(3) C25 0.060(4) 0.058(4) 0.071(5) -0.004(4) 0.012(3) -0.012(3) C26 0.060(4) 0.080(5) 0.058(4) -0.025(4) 0.004(3) -0.003(4) C27 0.079(5) 0.083(5) 0.041(3) -0.004(4) 0.008(3) -0.006(4) C28 0.070(4) 0.061(4) 0.042(3) 0.003(3) 0.014(3) -0.007(3) C29 0.049(3) 0.041(3) 0.046(3) 0.003(3) 0.005(3) -0.004(3) C30 0.068(4) 0.064(4) 0.063(4) 0.019(3) 0.029(3) 0.011(3) C31 0.125(7) 0.086(6) 0.080(5) 0.036(5) 0.056(5) 0.023(5) C32 0.111(7) 0.085(6) 0.071(5) 0.040(4) 0.022(5) 0.009(5) C33 0.064(4) 0.071(5) 0.086(5) 0.031(4) -0.006(4) 0.005(4) C34 0.053(4) 0.063(4) 0.064(4) 0.014(3) 0.006(3) -0.001(3) C35 0.053(4) 0.077(5) 0.076(5) 0.009(4) 0.019(4) 0.012(4) C36 0.083(6) 0.139(8) 0.138(8) 0.064(7) 0.048(6) -0.006(6) P3 0.0839(14) 0.0705(13) 0.0598(11) 0.0076(10) 0.0180(10) 0.0077(11) F1 0.326(13) 0.330(13) 0.342(12) 0.189(11) 0.271(11) 0.092(11) F2 0.258(11) 0.122(6) 0.399(14) -0.079(8) -0.005(11) -0.042(7) F3 0.288(10) 0.182(7) 0.219(8) 0.007(6) 0.174(8) 0.010(7) F4 0.250(10) 0.206(8) 0.298(11) -0.175(8) 0.032(9) -0.009(8) F5 0.151(7) 0.256(9) 0.309(10) 0.155(9) -0.084(7) 0.016(6) F6 0.196(9) 0.233(9) 0.309(12) 0.095(9) -0.045(8) 0.065(8) _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 N1 2.040(5) . ? Ru1 C3 2.181(6) . ? Ru1 C2 2.197(6) . ? Ru1 C4 2.210(6) . ? Ru1 C5 2.223(6) . ? Ru1 C1 2.250(6) . ? Ru1 P2 2.3142(17) . ? Ru1 P1 2.3161(16) . ? P1 C21 1.812(6) . ? P1 C23 1.835(6) . ? P1 C29 1.835(6) . ? P2 C7 1.811(6) . ? P2 C9 1.837(6) . ? P2 C15 1.840(6) . ? N1 C35 1.135(7) . ? C1 C2 1.408(10) . ? C1 C5 1.418(10) . ? C1 C6 1.500(10) . ? C2 C3 1.414(9) . ? C3 C4 1.400(9) . ? C4 C5 1.378(9) . ? C7 C8 1.304(9) . ? C9 C14 1.378(9) . ? C9 C10 1.385(9) . ? C10 C11 1.386(10) . ? C11 C12 1.393(11) . ? C12 C13 1.351(10) . ? C13 C14 1.402(9) . ? C15 C16 1.380(8) . ? C15 C20 1.389(8) . ? C16 C17 1.384(9) . ? C17 C18 1.362(10) . ? C18 C19 1.368(10) . ? C19 C20 1.379(9) . ? C21 C22 1.283(8) . ? C23 C24 1.384(8) . ? C23 C28 1.397(7) . ? C24 C25 1.366(8) . ? C25 C26 1.376(9) . ? C26 C27 1.381(9) . ? C27 C28 1.361(8) . ? C29 C34 1.377(8) . ? C29 C30 1.386(8) . ? C30 C31 1.375(9) . ? C31 C32 1.370(10) . ? C32 C33 1.363(10) . ? C33 C34 1.375(8) . ? C35 C36 1.469(10) . ? P3 F1 1.440(6) . ? P3 F5 1.454(6) . ? P3 F2 1.486(8) . ? P3 F4 1.486(7) . ? P3 F3 1.500(7) . ? P3 F6 1.530(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 N1 Ru1 C3 156.3(2) . . ? N1 Ru1 C2 134.2(3) . . ? C3 Ru1 C2 37.7(2) . . ? N1 Ru1 C4 121.6(2) . . ? C3 Ru1 C4 37.2(2) . . ? C2 Ru1 C4 62.0(3) . . ? N1 Ru1 C5 94.9(2) . . ? C3 Ru1 C5 61.4(3) . . ? C2 Ru1 C5 61.3(3) . . ? C4 Ru1 C5 36.2(2) . . ? N1 Ru1 C1 100.4(2) . . ? C3 Ru1 C1 62.3(3) . . ? C2 Ru1 C1 36.9(3) . . ? C4 Ru1 C1 61.7(3) . . ? C5 Ru1 C1 36.9(3) . . ? N1 Ru1 P2 91.72(15) . . ? C3 Ru1 P2 97.4(2) . . ? C2 Ru1 P2 133.4(2) . . ? C4 Ru1 P2 89.5(2) . . ? C5 Ru1 P2 116.4(2) . . ? C1 Ru1 P2 151.0(2) . . ? N1 Ru1 P1 88.11(14) . . ? C3 Ru1 P1 112.3(2) . . ? C2 Ru1 P1 93.12(19) . . ? C4 Ru1 P1 149.49(19) . . ? C5 Ru1 P1 146.4(2) . . ? C1 Ru1 P1 109.6(2) . . ? P2 Ru1 P1 96.89(6) . . ? C21 P1 C23 104.5(3) . . ? C21 P1 C29 100.7(3) . . ? C23 P1 C29 103.1(3) . . ? C21 P1 Ru1 116.9(2) . . ? C23 P1 Ru1 110.92(18) . . ? C29 P1 Ru1 118.90(19) . . ? C7 P2 C9 103.6(3) . . ? C7 P2 C15 103.9(3) . . ? C9 P2 C15 101.4(3) . . ? C7 P2 Ru1 110.9(2) . . ? C9 P2 Ru1 115.5(2) . . ? C15 P2 Ru1 119.67(19) . . ? C35 N1 Ru1 173.1(5) . . ? C2 C1 C5 105.9(6) . . ? C2 C1 C6 127.8(9) . . ? C5 C1 C6 125.9(9) . . ? C2 C1 Ru1 69.5(4) . . ? C5 C1 Ru1 70.5(4) . . ? C6 C1 Ru1 130.1(5) . . ? C1 C2 C3 108.7(6) . . ? C1 C2 Ru1 73.6(4) . . ? C3 C2 Ru1 70.5(4) . . ? C4 C3 C2 107.5(7) . . ? C4 C3 Ru1 72.5(4) . . ? C2 C3 Ru1 71.8(4) . . ? C5 C4 C3 108.1(7) . . ? C5 C4 Ru1 72.4(4) . . ? C3 C4 Ru1 70.3(4) . . ? C4 C5 C1 109.8(7) . . ? C4 C5 Ru1 71.4(4) . . ? C1 C5 Ru1 72.6(4) . . ? C8 C7 P2 126.8(6) . . ? C14 C9 C10 118.9(6) . . ? C14 C9 P2 120.3(5) . . ? C10 C9 P2 120.8(5) . . ? C9 C10 C11 121.2(8) . . ? C10 C11 C12 118.7(8) . . ? C13 C12 C11 120.8(7) . . ? C12 C13 C14 120.2(8) . . ? C9 C14 C13 120.2(7) . . ? C16 C15 C20 118.2(6) . . ? C16 C15 P2 119.5(4) . . ? C20 C15 P2 122.0(5) . . ? C15 C16 C17 121.3(6) . . ? C18 C17 C16 119.6(7) . . ? C17 C18 C19 120.0(7) . . ? C18 C19 C20 120.7(7) . . ? C19 C20 C15 120.1(6) . . ? C22 C21 P1 129.7(5) . . ? C24 C23 C28 118.1(5) . . ? C24 C23 P1 123.1(4) . . ? C28 C23 P1 118.8(4) . . ? C25 C24 C23 120.8(6) . . ? C24 C25 C26 120.5(6) . . ? C25 C26 C27 119.4(6) . . ? C28 C27 C26 120.2(6) . . ? C27 C28 C23 120.9(6) . . ? C34 C29 C30 118.7(5) . . ? C34 C29 P1 121.7(4) . . ? C30 C29 P1 119.6(5) . . ? C31 C30 C29 119.9(6) . . ? C32 C31 C30 120.4(7) . . ? C33 C32 C31 120.4(7) . . ? C32 C33 C34 119.5(7) . . ? C33 C34 C29 121.1(6) . . ? N1 C35 C36 177.0(8) . . ? F1 P3 F5 90.1(6) . . ? F1 P3 F2 90.8(7) . . ? F5 P3 F2 96.9(6) . . ? F1 P3 F4 93.5(7) . . ? F5 P3 F4 88.3(6) . . ? F2 P3 F4 173.2(6) . . ? F1 P3 F3 177.5(7) . . ? F5 P3 F3 91.8(5) . . ? F2 P3 F3 90.6(6) . . ? F4 P3 F3 84.9(5) . . ? F1 P3 F6 93.2(6) . . ? F5 P3 F6 176.5(6) . . ? F2 P3 F6 84.0(6) . . ? F4 P3 F6 90.5(6) . . ? F3 P3 F6 84.9(6) . . ? _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.895 _refine_diff_density_max 0.672 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.076 #===END data_jhn473a _database_code_CSD 195527 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 5 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H47 F6 P4 Ru' _chemical_formula_weight 962.81 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' 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 P2(1)/c 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 15.716(4) _cell_length_b 13.605(2) _cell_length_c 20.704(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.081(19) _cell_angle_gamma 90.00 _cell_volume 4392.9(17) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 18 _cell_measurement_theta_min 4.83 _cell_measurement_theta_max 12.21 _exptl_crystal_description block _exptl_crystal_colour red-violet _exptl_crystal_size_max .28 _exptl_crystal_size_mid .42 _exptl_crystal_size_min .38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1972 _exptl_absorpt_coefficient_mu 0.562 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8457 _exptl_absorpt_correction_T_max 0.9791 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7085 _diffrn_reflns_av_R_equivalents 0.1059 _diffrn_reflns_av_sigmaI/netI 0.1875 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5715 _reflns_number_gt 2945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1053P)^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_number_reflns 5715 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1803 _refine_ls_R_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.2418 _refine_ls_wR_factor_gt 0.1913 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.71599(7) 0.36694(7) 0.82074(5) 0.0331(4) Uani 1 1 d . . . P1 P 0.8439(2) 0.4158(3) 0.88440(19) 0.0469(10) Uani 1 1 d . . . P2 P 0.6281(2) 0.4073(3) 0.90059(17) 0.0387(9) Uani 1 1 d . . . P3 P 0.6958(2) 0.5173(3) 0.76379(18) 0.0421(10) Uani 1 1 d . . . C1 C 0.7767(9) 0.2328(13) 0.7764(9) 0.065(5) Uani 1 1 d . . . C2 C 0.7144(13) 0.2801(10) 0.7281(7) 0.063(5) Uani 1 1 d . . . H2A H 0.7252 0.3056 0.6856 0.076 Uiso 1 1 calc R . . C3 C 0.6353(10) 0.2744(12) 0.7517(8) 0.058(4) Uani 1 1 d . . . H3A H 0.5798 0.2930 0.7279 0.069 Uiso 1 1 calc R . . C4 C 0.6481(12) 0.2241(10) 0.8116(9) 0.069(5) Uani 1 1 d . . . H4A H 0.6034 0.2020 0.8374 0.083 Uiso 1 1 calc R . . C5 C 0.7321(10) 0.2036(11) 0.8233(10) 0.075(6) Uani 1 1 d . . . H5A H 0.7576 0.1679 0.8620 0.090 Uiso 1 1 calc R . . C6 C 0.8622(12) 0.2051(19) 0.7662(12) 0.143(10) Uani 1 1 d . . . H6A H 0.8610 0.1417 0.7458 0.214 Uiso 1 1 calc R . . H6B H 0.8978 0.2024 0.8073 0.214 Uiso 1 1 calc R . . H6C H 0.8848 0.2528 0.7387 0.214 Uiso 1 1 calc R . . C7 C 0.8518(9) 0.5421(10) 0.9142(7) 0.056(4) Uani 1 1 d . . . H7A H 0.8101 0.5631 0.9392 0.067 Uiso 1 1 calc R . . C8 C 0.9114(10) 0.6061(11) 0.9033(9) 0.086(6) Uani 1 1 d . . . H8A H 0.9543 0.5881 0.8785 0.103 Uiso 1 1 calc R . . H8B H 0.9104 0.6692 0.9205 0.103 Uiso 1 1 calc R . . C9 C 0.8707(9) 0.3455(10) 0.9601(8) 0.055(4) Uani 1 1 d . . . C10 C 0.8982(10) 0.2474(11) 0.9564(8) 0.072(5) Uani 1 1 d . . . H10A H 0.9048 0.2179 0.9168 0.086 Uiso 1 1 calc R . . C11 C 0.9149(10) 0.1968(12) 1.0149(9) 0.073(5) Uani 1 1 d . . . H11A H 0.9347 0.1325 1.0135 0.088 Uiso 1 1 calc R . . C12 C 0.9043(12) 0.2342(14) 1.0732(9) 0.086(6) Uani 1 1 d . . . H12A H 0.9171 0.1970 1.1109 0.103 Uiso 1 1 calc R . . C13 C 0.8737(10) 0.3298(14) 1.0762(9) 0.071(5) Uani 1 1 d . . . H13A H 0.8640 0.3569 1.1159 0.085 Uiso 1 1 calc R . . C14 C 0.8578(9) 0.3842(11) 1.0196(8) 0.060(4) Uani 1 1 d . . . H14A H 0.8380 0.4484 1.0217 0.072 Uiso 1 1 calc R . . C15 C 0.9464(9) 0.4048(10) 0.8484(9) 0.058(4) Uani 1 1 d . . . C16 C 0.9467(10) 0.4136(11) 0.7827(8) 0.057(4) Uani 1 1 d . . . H16A H 0.8953 0.4167 0.7552 0.068 Uiso 1 1 calc R . . C17 C 1.0251(12) 0.4178(13) 0.7572(11) 0.089(6) Uani 1 1 d . . . H17A H 1.0272 0.4274 0.7129 0.107 Uiso 1 1 calc R . . C18 C 1.0991(12) 0.4074(15) 0.7997(14) 0.105(8) Uani 1 1 d . . . H18A H 1.1509 0.4045 0.7825 0.126 Uiso 1 1 calc R . . C19 C 1.1008(12) 0.4013(16) 0.8627(12) 0.098(8) Uani 1 1 d . . . H19A H 1.1532 0.3989 0.8890 0.118 Uiso 1 1 calc R . . C20 C 1.0240(10) 0.3983(12) 0.8909(11) 0.093(7) Uani 1 1 d . . . H20A H 1.0251 0.4518 0.9220 0.111 Uiso 1 1 calc R . . H20B H 1.0231 0.3375 0.9153 0.111 Uiso 1 1 calc R . . C21 C 0.6503(8) 0.5160(10) 0.9505(6) 0.041(4) Uani 1 1 d . . . H21A H 0.6503 0.5756 0.9284 0.050 Uiso 1 1 calc R . . C22 C 0.6662(9) 0.5205(12) 1.0128(7) 0.062(5) Uani 1 1 d . . . H22A H 0.6672 0.4633 1.0374 0.075 Uiso 1 1 calc R . . H22B H 0.6768 0.5809 1.0332 0.075 Uiso 1 1 calc R . . C23 C 0.6147(9) 0.3140(9) 0.9629(7) 0.047(4) Uani 1 1 d . . . C24 C 0.5438(9) 0.3153(11) 0.9982(7) 0.055(4) Uani 1 1 d . . . H24A H 0.5022 0.3635 0.9889 0.066 Uiso 1 1 calc R . . C25 C 0.5337(10) 0.2473(11) 1.0464(7) 0.056(4) Uani 1 1 d . . . H25A H 0.4865 0.2502 1.0693 0.067 Uiso 1 1 calc R . . C26 C 0.5950(10) 0.1751(11) 1.0598(7) 0.056(4) Uani 1 1 d . . . H26A H 0.5897 0.1291 1.0922 0.067 Uiso 1 1 calc R . . C27 C 0.6646(10) 0.1715(11) 1.0246(7) 0.053(4) Uani 1 1 d . . . H27A H 0.7047 0.1214 1.0328 0.064 Uiso 1 1 calc R . . C28 C 0.6755(9) 0.2416(10) 0.9773(6) 0.048(4) Uani 1 1 d . . . H28A H 0.7237 0.2396 0.9555 0.058 Uiso 1 1 calc R . . C29 C 0.5158(8) 0.4312(9) 0.8679(7) 0.041(3) Uani 1 1 d . . . C30 C 0.4832(9) 0.5246(10) 0.8629(7) 0.054(4) Uani 1 1 d . . . H30A H 0.5171 0.5770 0.8795 0.065 Uiso 1 1 calc R . . C31 C 0.3993(10) 0.5428(12) 0.8331(8) 0.064(5) Uani 1 1 d . . . H31A H 0.3790 0.6071 0.8295 0.077 Uiso 1 1 calc R . . C32 C 0.3481(12) 0.4682(15) 0.8099(8) 0.079(5) Uani 1 1 d . . . H32A H 0.2934 0.4806 0.7889 0.095 Uiso 1 1 calc R . . C33 C 0.3776(10) 0.3745(14) 0.8177(8) 0.073(5) Uani 1 1 d . . . H33A H 0.3410 0.3230 0.8037 0.088 Uiso 1 1 calc R . . C34 C 0.4622(8) 0.3525(11) 0.8463(7) 0.057(4) Uani 1 1 d . . . H34A H 0.4815 0.2880 0.8506 0.068 Uiso 1 1 calc R . . C35 C 0.6824(10) 0.6300(10) 0.8060(7) 0.051(4) Uani 1 1 d . . . H35A H 0.7281 0.6495 0.8361 0.061 Uiso 1 1 calc R . . C36 C 0.6161(11) 0.6875(11) 0.7993(7) 0.062(4) Uani 1 1 d . . . H36A H 0.5685 0.6716 0.7699 0.074 Uiso 1 1 calc R . . H36B H 0.6161 0.7447 0.8240 0.074 Uiso 1 1 calc R . . C37 C 0.6057(10) 0.5214(9) 0.6974(6) 0.044(4) Uani 1 1 d . . . C38 C 0.5279(10) 0.4742(11) 0.7067(7) 0.055(4) Uani 1 1 d . . . H38A H 0.5228 0.4399 0.7449 0.066 Uiso 1 1 calc R . . C39 C 0.4600(11) 0.4801(11) 0.6582(8) 0.062(5) Uani 1 1 d . . . H39A H 0.4103 0.4454 0.6633 0.074 Uiso 1 1 calc R . . C40 C 0.4619(12) 0.5313(14) 0.6063(10) 0.079(6) Uani 1 1 d . . . H40A H 0.4134 0.5341 0.5757 0.094 Uiso 1 1 calc R . . C41 C 0.5355(16) 0.5830(12) 0.5950(8) 0.086(6) Uani 1 1 d . . . H41A H 0.5373 0.6197 0.5573 0.103 Uiso 1 1 calc R . . C42 C 0.6070(11) 0.5770(10) 0.6433(8) 0.067(5) Uani 1 1 d . . . H42A H 0.6564 0.6121 0.6378 0.081 Uiso 1 1 calc R . . C43 C 0.7819(9) 0.5513(10) 0.7176(7) 0.047(4) Uani 1 1 d . . . C44 C 0.7961(11) 0.5044(12) 0.6606(8) 0.066(5) Uani 1 1 d . . . H44A H 0.7596 0.4527 0.6469 0.080 Uiso 1 1 calc R . . C45 C 0.8586(13) 0.5268(13) 0.6224(10) 0.092(6) Uani 1 1 d . . . H45A H 0.8632 0.4922 0.5842 0.110 Uiso 1 1 calc R . . C46 C 0.9141(14) 0.6016(14) 0.6422(12) 0.105(8) Uani 1 1 d . . . H46A H 0.9577 0.6185 0.6177 0.126 Uiso 1 1 calc R . . C47 C 0.9049(14) 0.6509(14) 0.6983(11) 0.104(7) Uani 1 1 d . . . H47A H 0.9441 0.6997 0.7129 0.124 Uiso 1 1 calc R . . C48 C 0.8369(10) 0.6291(11) 0.7346(8) 0.065(4) Uani 1 1 d . . . H48A H 0.8289 0.6677 0.7705 0.077 Uiso 1 1 calc R . . P4 P 0.8164(4) 0.9159(5) 0.9021(3) 0.103(2) Uani 1 1 d . . . F6 F 0.8681(13) 0.8438(11) 0.8678(8) 0.206(8) Uani 1 1 d . . . F4 F 0.8581(11) 0.8811(17) 0.9678(7) 0.213(9) Uani 1 1 d . . . F3 F 0.7658(11) 0.9917(13) 0.9367(9) 0.198(8) Uani 1 1 d . . . F2 F 0.7670(13) 0.9464(19) 0.8397(8) 0.252(11) Uani 1 1 d . . . F5 F 0.8877(14) 0.9881(16) 0.8928(15) 0.296(14) Uani 1 1 d . . . F1 F 0.7476(14) 0.8412(15) 0.9182(11) 0.239(10) Uani 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 Ru1 0.0340(6) 0.0239(6) 0.0398(6) -0.0003(6) -0.0016(4) -0.0008(6) P1 0.044(2) 0.041(2) 0.054(3) -0.007(2) -0.0004(19) -0.0002(19) P2 0.043(2) 0.031(2) 0.041(2) -0.0013(17) 0.0018(17) 0.0021(17) P3 0.049(2) 0.030(2) 0.047(2) 0.0027(18) 0.0022(19) 0.0004(18) C1 0.026(9) 0.076(13) 0.097(14) -0.041(11) 0.022(9) 0.005(9) C2 0.138(17) 0.021(8) 0.030(8) -0.009(7) 0.009(10) -0.010(10) C3 0.050(10) 0.059(11) 0.061(11) -0.021(10) -0.004(9) -0.008(9) C4 0.090(14) 0.024(8) 0.095(14) -0.020(9) 0.020(11) -0.027(9) C5 0.045(12) 0.047(11) 0.125(17) -0.045(11) -0.020(12) 0.023(9) C6 0.089(17) 0.15(2) 0.19(3) -0.03(2) 0.046(17) 0.005(16) C7 0.048(9) 0.043(9) 0.071(11) -0.003(8) -0.010(8) -0.007(8) C8 0.066(12) 0.047(11) 0.141(18) 0.004(11) -0.004(11) -0.017(9) C9 0.055(9) 0.034(9) 0.066(11) -0.011(8) -0.035(8) 0.002(7) C10 0.081(12) 0.051(11) 0.077(12) 0.002(10) -0.016(10) 0.016(9) C11 0.076(12) 0.058(11) 0.074(12) -0.003(11) -0.038(10) 0.025(9) C12 0.103(15) 0.080(14) 0.057(12) -0.001(11) -0.062(11) 0.001(12) C13 0.065(11) 0.072(13) 0.068(12) -0.005(10) -0.017(9) 0.000(10) C14 0.065(10) 0.037(10) 0.071(12) 0.005(9) -0.014(9) -0.010(8) C15 0.045(10) 0.041(9) 0.086(13) -0.010(9) -0.003(9) -0.018(7) C16 0.052(10) 0.048(9) 0.073(12) 0.005(9) 0.022(9) -0.016(8) C17 0.064(13) 0.074(13) 0.132(18) 0.034(13) 0.022(13) -0.019(10) C18 0.039(12) 0.096(16) 0.18(3) -0.025(18) 0.021(16) -0.009(11) C19 0.056(13) 0.121(19) 0.115(18) -0.063(16) 0.000(13) -0.013(12) C20 0.043(11) 0.055(12) 0.18(2) -0.029(12) 0.002(12) 0.006(9) C21 0.045(9) 0.042(9) 0.034(9) 0.000(7) -0.006(7) -0.002(7) C22 0.074(12) 0.058(11) 0.054(11) -0.023(9) 0.003(9) -0.003(9) C23 0.060(10) 0.020(7) 0.057(10) -0.003(7) -0.007(8) 0.004(7) C24 0.050(10) 0.049(10) 0.068(11) -0.013(9) 0.016(8) 0.009(8) C25 0.070(11) 0.056(10) 0.046(9) 0.007(9) 0.028(8) -0.013(9) C26 0.065(11) 0.035(9) 0.064(11) 0.007(8) -0.005(9) -0.028(9) C27 0.051(10) 0.043(9) 0.059(10) -0.003(8) -0.018(8) 0.001(8) C28 0.058(9) 0.050(10) 0.035(8) -0.010(8) 0.001(7) -0.012(8) C29 0.038(8) 0.026(8) 0.058(9) 0.003(7) 0.001(7) 0.005(7) C30 0.050(10) 0.040(9) 0.069(11) -0.009(8) -0.006(8) 0.001(8) C31 0.053(11) 0.047(10) 0.089(13) 0.009(10) -0.004(9) 0.009(9) C32 0.072(13) 0.090(15) 0.071(12) 0.001(11) -0.014(10) 0.019(12) C33 0.050(10) 0.085(14) 0.081(12) -0.022(12) -0.006(9) -0.005(11) C34 0.041(9) 0.048(10) 0.074(11) -0.017(9) -0.018(8) 0.005(8) C35 0.069(10) 0.023(7) 0.059(10) -0.006(8) -0.001(8) 0.001(8) C36 0.091(13) 0.034(9) 0.064(11) -0.002(8) 0.024(10) -0.006(9) C37 0.072(11) 0.021(7) 0.039(8) 0.002(7) 0.007(8) 0.001(7) C38 0.069(11) 0.049(10) 0.045(9) -0.002(8) -0.003(9) 0.013(9) C39 0.084(12) 0.048(10) 0.047(10) 0.001(9) -0.018(9) 0.005(9) C40 0.076(14) 0.057(12) 0.095(16) -0.015(12) -0.021(12) 0.042(11) C41 0.15(2) 0.041(10) 0.057(11) 0.026(9) -0.019(13) 0.043(12) C42 0.080(12) 0.025(8) 0.089(13) 0.010(9) -0.020(10) -0.003(8) C43 0.054(9) 0.032(8) 0.051(10) 0.006(7) -0.004(8) -0.015(7) C44 0.101(14) 0.050(10) 0.052(11) 0.010(9) 0.024(10) -0.007(10) C45 0.111(16) 0.058(13) 0.120(17) -0.010(12) 0.070(14) -0.005(12) C46 0.110(17) 0.062(14) 0.15(2) 0.015(14) 0.062(17) -0.034(12) C47 0.131(19) 0.057(14) 0.131(19) -0.001(13) 0.049(16) -0.034(13) C48 0.072(11) 0.043(9) 0.078(11) 0.011(10) 0.008(9) -0.003(10) P4 0.104(5) 0.092(4) 0.106(5) -0.019(4) -0.016(4) 0.027(4) F6 0.33(2) 0.119(12) 0.183(15) 0.003(11) 0.090(16) 0.105(15) F4 0.175(15) 0.36(3) 0.099(10) -0.009(14) -0.016(10) 0.111(18) F3 0.208(17) 0.180(16) 0.211(17) -0.052(13) 0.049(13) 0.093(14) F2 0.210(18) 0.37(3) 0.148(14) -0.057(18) -0.079(13) 0.12(2) F5 0.23(2) 0.22(2) 0.47(4) -0.07(2) 0.15(3) -0.120(19) F1 0.27(2) 0.194(19) 0.26(2) 0.002(17) 0.06(2) -0.112(18) _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 C3 2.188(14) . ? Ru1 C4 2.213(14) . ? Ru1 C5 2.236(15) . ? Ru1 C2 2.250(13) . ? Ru1 C1 2.303(15) . ? Ru1 P2 2.347(4) . ? Ru1 P1 2.359(4) . ? Ru1 P3 2.362(4) . ? P1 C7 1.824(15) . ? P1 C9 1.840(15) . ? P1 C15 1.862(16) . ? P2 C21 1.813(13) . ? P2 C29 1.839(13) . ? P2 C23 1.841(14) . ? P3 C35 1.791(14) . ? P3 C43 1.810(15) . ? P3 C37 1.849(14) . ? C1 C5 1.33(2) . ? C1 C6 1.43(2) . ? C1 C2 1.46(2) . ? C2 C3 1.39(2) . ? C3 C4 1.41(2) . ? C4 C5 1.34(2) . ? C7 C8 1.318(19) . ? C9 C14 1.38(2) . ? C9 C10 1.409(19) . ? C10 C11 1.39(2) . ? C11 C12 1.34(2) . ? C12 C13 1.39(2) . ? C13 C14 1.38(2) . ? C15 C16 1.37(2) . ? C15 C20 1.42(2) . ? C16 C17 1.40(2) . ? C17 C18 1.38(3) . ? C18 C19 1.30(3) . ? C19 C20 1.41(2) . ? C21 C22 1.284(17) . ? C23 C28 1.378(18) . ? C23 C24 1.407(18) . ? C24 C25 1.383(19) . ? C25 C26 1.379(19) . ? C26 C27 1.387(19) . ? C27 C28 1.393(18) . ? C29 C30 1.369(18) . ? C29 C34 1.400(18) . ? C30 C31 1.406(19) . ? C31 C32 1.35(2) . ? C32 C33 1.36(2) . ? C33 C34 1.420(19) . ? C35 C36 1.297(18) . ? C37 C42 1.353(19) . ? C37 C38 1.415(19) . ? C38 C39 1.374(19) . ? C39 C40 1.28(2) . ? C40 C41 1.40(2) . ? C41 C42 1.41(2) . ? C43 C48 1.385(19) . ? C43 C44 1.383(19) . ? C44 C45 1.37(2) . ? C45 C46 1.37(2) . ? C46 C47 1.36(3) . ? C47 C48 1.41(2) . ? P4 F2 1.483(17) . ? P4 F6 1.506(14) . ? P4 F4 1.512(15) . ? P4 F5 1.519(18) . ? P4 F3 1.533(14) . ? P4 F1 1.551(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Ru1 C4 37.4(6) . . ? C3 Ru1 C5 59.9(6) . . ? C4 Ru1 C5 35.1(5) . . ? C3 Ru1 C2 36.5(5) . . ? C4 Ru1 C2 60.8(6) . . ? C5 Ru1 C2 59.2(6) . . ? C3 Ru1 C1 61.3(6) . . ? C4 Ru1 C1 59.3(6) . . ? C5 Ru1 C1 33.9(6) . . ? C2 Ru1 C1 37.4(5) . . ? C3 Ru1 P2 104.5(5) . . ? C4 Ru1 P2 86.9(5) . . ? C5 Ru1 P2 106.9(6) . . ? C2 Ru1 P2 141.0(5) . . ? C1 Ru1 P2 140.8(5) . . ? C3 Ru1 P1 155.8(4) . . ? C4 Ru1 P1 131.6(5) . . ? C5 Ru1 P1 100.4(4) . . ? C2 Ru1 P1 122.9(5) . . ? C1 Ru1 P1 94.6(4) . . ? P2 Ru1 P1 94.33(13) . . ? C3 Ru1 P3 98.1(5) . . ? C4 Ru1 P3 133.1(5) . . ? C5 Ru1 P3 151.6(5) . . ? C2 Ru1 P3 92.4(4) . . ? C1 Ru1 P3 121.6(5) . . ? P2 Ru1 P3 95.41(13) . . ? P1 Ru1 P3 95.02(14) . . ? C7 P1 C9 101.7(6) . . ? C7 P1 C15 100.7(7) . . ? C9 P1 C15 100.4(7) . . ? C7 P1 Ru1 118.2(5) . . ? C9 P1 Ru1 114.8(5) . . ? C15 P1 Ru1 118.2(5) . . ? C21 P2 C29 100.1(6) . . ? C21 P2 C23 101.2(6) . . ? C29 P2 C23 101.1(6) . . ? C21 P2 Ru1 120.2(5) . . ? C29 P2 Ru1 113.8(5) . . ? C23 P2 Ru1 117.4(5) . . ? C35 P3 C43 100.4(7) . . ? C35 P3 C37 102.2(6) . . ? C43 P3 C37 98.8(6) . . ? C35 P3 Ru1 121.0(5) . . ? C43 P3 Ru1 114.9(5) . . ? C37 P3 Ru1 116.2(4) . . ? C5 C1 C6 128(2) . . ? C5 C1 C2 105.2(14) . . ? C6 C1 C2 125(2) . . ? C5 C1 Ru1 70.3(9) . . ? C6 C1 Ru1 135.1(14) . . ? C2 C1 Ru1 69.3(8) . . ? C3 C2 C1 106.7(14) . . ? C3 C2 Ru1 69.3(8) . . ? C1 C2 Ru1 73.3(8) . . ? C2 C3 C4 107.4(15) . . ? C2 C3 Ru1 74.1(8) . . ? C4 C3 Ru1 72.3(8) . . ? C5 C4 C3 106.9(17) . . ? C5 C4 Ru1 73.4(9) . . ? C3 C4 Ru1 70.4(8) . . ? C1 C5 C4 113.8(19) . . ? C1 C5 Ru1 75.8(11) . . ? C4 C5 Ru1 71.5(9) . . ? C8 C7 P1 125.8(14) . . ? C14 C9 C10 119.4(15) . . ? C14 C9 P1 121.3(11) . . ? C10 C9 P1 119.1(13) . . ? C11 C10 C9 116.6(16) . . ? C12 C11 C10 124.5(16) . . ? C11 C12 C13 118.5(17) . . ? C14 C13 C12 119.3(17) . . ? C9 C14 C13 121.5(15) . . ? C16 C15 C20 121.0(16) . . ? C16 C15 P1 120.1(12) . . ? C20 C15 P1 118.5(14) . . ? C15 C16 C17 119.4(16) . . ? C18 C17 C16 118(2) . . ? C19 C18 C17 124(2) . . ? C18 C19 C20 120(2) . . ? C19 C20 C15 117.2(19) . . ? C22 C21 P2 127.6(12) . . ? C28 C23 C24 117.9(13) . . ? C28 C23 P2 120.6(12) . . ? C24 C23 P2 121.4(11) . . ? C25 C24 C23 122.3(14) . . ? C24 C25 C26 118.8(14) . . ? C25 C26 C27 119.7(14) . . ? C26 C27 C28 121.2(14) . . ? C23 C28 C27 120.0(14) . . ? C30 C29 C34 118.7(13) . . ? C30 C29 P2 121.7(10) . . ? C34 C29 P2 119.6(10) . . ? C29 C30 C31 121.2(14) . . ? C32 C31 C30 120.7(15) . . ? C31 C32 C33 119.0(16) . . ? C32 C33 C34 122.4(16) . . ? C29 C34 C33 117.8(14) . . ? C36 C35 P3 127.3(12) . . ? C42 C37 C38 117.9(14) . . ? C42 C37 P3 122.9(12) . . ? C38 C37 P3 118.7(10) . . ? C39 C38 C37 118.7(15) . . ? C40 C39 C38 123.2(18) . . ? C39 C40 C41 121.2(17) . . ? C40 C41 C42 117.1(16) . . ? C37 C42 C41 121.7(17) . . ? C48 C43 C44 114.1(15) . . ? C48 C43 P3 123.0(12) . . ? C44 C43 P3 122.8(11) . . ? C45 C44 C43 126.4(17) . . ? C44 C45 C46 117.9(19) . . ? C47 C46 C45 119.3(19) . . ? C46 C47 C48 121.1(19) . . ? C43 C48 C47 121.0(17) . . ? F2 P4 F6 91.5(11) . . ? F2 P4 F4 174.0(14) . . ? F6 P4 F4 91.3(9) . . ? F2 P4 F5 91.4(16) . . ? F6 P4 F5 85.0(12) . . ? F4 P4 F5 94.2(14) . . ? F2 P4 F3 88.4(10) . . ? F6 P4 F3 178.3(12) . . ? F4 P4 F3 89.0(10) . . ? F5 P4 F3 93.3(12) . . ? F2 P4 F1 93.8(13) . . ? F6 P4 F1 96.1(12) . . ? F4 P4 F1 80.6(12) . . ? F5 P4 F1 174.7(16) . . ? F3 P4 F1 85.7(11) . . ? _diffrn_measured_fraction_theta_max 0.843 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.843 _refine_diff_density_max 0.826 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.117 #===END data_jhn435b _database_code_CSD 195528 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 7 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H39 F6 O P3 Ru' _chemical_formula_weight 807.66 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' O O 0.0106 0.0060 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 13.6771(19) _cell_length_b 13.6771(19) _cell_length_c 39.271(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7346(2) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 4.90 _cell_measurement_theta_max 11.43 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max .12 _exptl_crystal_size_mid .48 _exptl_crystal_size_min .42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 0.617 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8984 _exptl_absorpt_correction_T_max 0.9819 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11567 _diffrn_reflns_av_R_equivalents 0.0871 _diffrn_reflns_av_sigmaI/netI 0.1125 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 22.51 _reflns_number_total 4807 _reflns_number_gt 3083 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0531P)^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 0.02(8) _refine_ls_number_reflns 4807 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1151 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Ru1 Ru 0.42052(6) 0.43996(6) 0.115740(19) 0.0457(2) Uani 1 1 d . . . P1 P 0.4859(2) 0.5240(2) 0.16152(7) 0.0552(8) Uani 1 1 d . . . P2 P 0.52327(19) 0.3061(2) 0.11872(8) 0.0512(8) Uani 1 1 d . . . C1 C 0.2916(9) 0.3915(11) 0.0824(4) 0.078(4) Uani 1 1 d . . . C2 C 0.2861(8) 0.4957(10) 0.0887(4) 0.070(4) Uani 1 1 d . . . H2A H 0.2847 0.5470 0.0713 0.084 Uiso 1 1 calc R . . C3 C 0.2748(7) 0.5098(9) 0.1237(3) 0.068(4) Uani 1 1 d . . . H3A H 0.2630 0.5725 0.1350 0.081 Uiso 1 1 calc R . . C4 C 0.2716(6) 0.4173(11) 0.1393(3) 0.068(3) Uani 1 1 d . . . H4A H 0.2580 0.4041 0.1633 0.082 Uiso 1 1 calc R . . C5 C 0.2834(7) 0.3468(9) 0.1134(3) 0.065(3) Uani 1 1 d . . . H5A H 0.2816 0.2759 0.1169 0.078 Uiso 1 1 calc R . . C6 C 0.2848(10) 0.3424(11) 0.0478(4) 0.126(6) Uani 1 1 d . . . H6A H 0.2173 0.3323 0.0420 0.190 Uiso 1 1 calc R . . H6B H 0.3179 0.2806 0.0485 0.190 Uiso 1 1 calc R . . H6C H 0.3149 0.3834 0.0309 0.190 Uiso 1 1 calc R . . C7 C 0.4099(8) 0.5026(9) 0.1985(2) 0.066(3) Uani 1 1 d . . . H7A H 0.4161 0.4424 0.2092 0.079 Uiso 1 1 calc R . . C8 C 0.3453(8) 0.5660(11) 0.2117(3) 0.099(5) Uani 1 1 d . . . H8A H 0.3368 0.6271 0.2017 0.119 Uiso 1 1 calc R . . H8B H 0.3091 0.5488 0.2308 0.119 Uiso 1 1 calc R . . C9 C 0.6079(7) 0.4962(9) 0.1779(3) 0.059(3) Uani 1 1 d . . . C10 C 0.6240(9) 0.4190(10) 0.1997(3) 0.082(4) Uani 1 1 d . . . H10A H 0.5711 0.3836 0.2080 0.099 Uiso 1 1 calc R . . C11 C 0.7175(11) 0.3934(12) 0.2094(4) 0.110(6) Uani 1 1 d . . . H11A H 0.7272 0.3428 0.2248 0.132 Uiso 1 1 calc R . . C12 C 0.7971(10) 0.4435(12) 0.1960(4) 0.098(5) Uani 1 1 d . . . H12A H 0.8601 0.4244 0.2018 0.117 Uiso 1 1 calc R . . C13 C 0.7835(9) 0.5203(10) 0.1744(3) 0.081(4) Uani 1 1 d . . . H13A H 0.8366 0.5544 0.1656 0.098 Uiso 1 1 calc R . . C14 C 0.6886(8) 0.5466(9) 0.1658(3) 0.077(4) Uani 1 1 d . . . H14A H 0.6789 0.5999 0.1515 0.092 Uiso 1 1 calc R . . C15 C 0.4866(7) 0.6570(8) 0.1576(3) 0.057(3) Uani 1 1 d . . . C16 C 0.4569(8) 0.7051(8) 0.1284(3) 0.067(3) Uani 1 1 d . . . H16A H 0.4351 0.6692 0.1097 0.080 Uiso 1 1 calc R . . C17 C 0.4595(8) 0.8061(9) 0.1267(4) 0.087(4) Uani 1 1 d . . . H17A H 0.4402 0.8375 0.1068 0.104 Uiso 1 1 calc R . . C18 C 0.4892(11) 0.8590(11) 0.1533(5) 0.107(6) Uani 1 1 d . . . H18A H 0.4887 0.9268 0.1519 0.128 Uiso 1 1 calc R . . C19 C 0.5208(10) 0.8143(12) 0.1828(4) 0.098(5) Uani 1 1 d . . . H19A H 0.5411 0.8518 0.2012 0.117 Uiso 1 1 calc R . . C20 C 0.5222(8) 0.7130(10) 0.1848(4) 0.083(4) Uani 1 1 d . . . H20A H 0.5468 0.6824 0.2041 0.099 Uiso 1 1 calc R . . C21 C 0.6530(7) 0.3284(8) 0.1158(3) 0.058(3) Uani 1 1 d . . . H21A H 0.6786 0.3713 0.1319 0.070 Uiso 1 1 calc R . . C22 C 0.7130(9) 0.2935(9) 0.0950(3) 0.091(4) Uani 1 1 d . . . H22A H 0.6920 0.2501 0.0784 0.109 Uiso 1 1 calc R . . H22B H 0.7786 0.3110 0.0963 0.109 Uiso 1 1 calc R . . C23 C 0.5162(8) 0.2283(8) 0.1566(3) 0.053(3) Uani 1 1 d . . . C24 C 0.4400(10) 0.2367(8) 0.1790(3) 0.071(3) Uani 1 1 d . . . H24A H 0.3909 0.2820 0.1746 0.085 Uiso 1 1 calc R . . C25 C 0.4339(12) 0.1794(10) 0.2081(4) 0.101(4) Uani 1 1 d . . . H25A H 0.3801 0.1841 0.2225 0.121 Uiso 1 1 calc R . . C26 C 0.5085(12) 0.1160(12) 0.2153(4) 0.113(6) Uani 1 1 d . . . H26A H 0.5070 0.0803 0.2354 0.135 Uiso 1 1 calc R . . C27 C 0.5839(12) 0.1043(9) 0.1937(4) 0.096(5) Uani 1 1 d . . . H27A H 0.6331 0.0592 0.1982 0.115 Uiso 1 1 calc R . . C28 C 0.5864(9) 0.1615(9) 0.1644(3) 0.080(4) Uani 1 1 d . . . H28A H 0.6385 0.1537 0.1494 0.096 Uiso 1 1 calc R . . C29 C 0.4967(8) 0.2194(8) 0.0844(3) 0.054(3) Uani 1 1 d . . . C30 C 0.4476(8) 0.1326(8) 0.0899(3) 0.066(3) Uani 1 1 d . . . H30A H 0.4310 0.1163 0.1122 0.079 Uiso 1 1 calc R . . C31 C 0.4217(8) 0.0685(9) 0.0641(3) 0.076(3) Uani 1 1 d . . . H31A H 0.3871 0.0112 0.0683 0.092 Uiso 1 1 calc R . . C32 C 0.4504(9) 0.0950(9) 0.0323(3) 0.076(4) Uani 1 1 d . . . H32A H 0.4360 0.0527 0.0144 0.091 Uiso 1 1 calc R . . C33 C 0.4979(9) 0.1778(11) 0.0250(3) 0.080(4) Uani 1 1 d . . . H33A H 0.5160 0.1917 0.0027 0.096 Uiso 1 1 calc R . . C34 C 0.5199(8) 0.2427(8) 0.0510(3) 0.066(3) Uani 1 1 d . . . H34A H 0.5503 0.3018 0.0461 0.079 Uiso 1 1 calc R . . C35 C 0.5108(7) 0.4979(7) 0.0842(2) 0.047(3) Uani 1 1 d . . . C36 C 0.4966(9) 0.5021(8) 0.0457(2) 0.093(4) Uani 1 1 d . . . H36A H 0.5515 0.5345 0.0354 0.139 Uiso 1 1 calc R . . H36B H 0.4379 0.5377 0.0406 0.139 Uiso 1 1 calc R . . H36C H 0.4914 0.4369 0.0368 0.139 Uiso 1 1 calc R . . C37 C 0.6535(11) 0.5965(13) 0.0696(4) 0.158(8) Uani 1 1 d . . . H37A H 0.7075 0.6249 0.0817 0.237 Uiso 1 1 calc R . . H37B H 0.6161 0.6473 0.0589 0.237 Uiso 1 1 calc R . . H37C H 0.6778 0.5525 0.0525 0.237 Uiso 1 1 calc R . . O1 O 0.5894(6) 0.5412(7) 0.09414(19) 0.094(3) Uani 1 1 d . . . P3 P 0.3682(3) 0.7703(3) 0.01574(9) 0.0769(10) Uani 1 1 d . . . F1 F 0.3219(12) 0.7381(13) 0.0478(3) 0.266(8) Uani 1 1 d . . . F2 F 0.3559(14) 0.6684(8) 0.0075(4) 0.285(9) Uani 1 1 d . . . F3 F 0.4134(10) 0.7983(18) -0.0150(3) 0.310(11) Uani 1 1 d . . . F4 F 0.3666(18) 0.8673(8) 0.0247(5) 0.316(11) Uani 1 1 d . . . F5 F 0.2713(9) 0.7830(12) -0.0027(4) 0.253(7) Uani 1 1 d . . . F6 F 0.4611(8) 0.7507(11) 0.0326(4) 0.246(7) Uani 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 Ru1 0.0405(5) 0.0508(5) 0.0458(4) -0.0004(4) 0.0024(4) 0.0014(5) P1 0.0510(19) 0.069(2) 0.0461(15) -0.0010(15) 0.0020(14) -0.0077(15) P2 0.0430(16) 0.0571(17) 0.0535(18) 0.0109(16) 0.0057(16) 0.0010(14) C1 0.067(9) 0.099(12) 0.067(10) -0.023(9) -0.007(7) 0.027(8) C2 0.048(8) 0.081(10) 0.082(10) 0.022(8) -0.011(7) 0.015(7) C3 0.045(7) 0.072(9) 0.085(11) -0.001(8) 0.003(7) 0.004(6) C4 0.022(5) 0.124(11) 0.058(7) -0.004(10) 0.007(5) 0.004(7) C5 0.047(7) 0.085(9) 0.063(8) 0.006(8) -0.008(7) 0.005(6) C6 0.096(11) 0.131(14) 0.152(16) -0.023(12) -0.023(11) 0.014(11) C7 0.061(7) 0.087(8) 0.050(6) 0.012(6) 0.006(6) -0.010(7) C8 0.070(8) 0.164(14) 0.063(8) -0.023(10) 0.019(7) 0.003(10) C9 0.050(7) 0.074(8) 0.053(7) 0.008(7) -0.007(6) -0.015(6) C10 0.071(9) 0.105(10) 0.070(8) 0.005(9) -0.015(7) -0.010(9) C11 0.091(11) 0.140(15) 0.099(11) 0.046(10) -0.035(10) -0.009(11) C12 0.068(9) 0.123(13) 0.103(12) -0.001(11) -0.039(9) -0.008(10) C13 0.055(8) 0.090(10) 0.099(11) 0.019(9) -0.002(8) -0.006(8) C14 0.056(8) 0.080(10) 0.094(9) 0.023(8) -0.010(7) -0.012(8) C15 0.041(7) 0.068(8) 0.060(7) -0.003(7) 0.021(6) -0.014(6) C16 0.065(8) 0.060(8) 0.074(9) -0.007(7) 0.001(7) -0.010(6) C17 0.065(9) 0.069(9) 0.126(13) 0.003(9) -0.003(9) 0.001(7) C18 0.079(11) 0.071(10) 0.171(18) -0.050(12) 0.004(12) 0.004(9) C19 0.081(11) 0.090(13) 0.122(14) -0.052(11) -0.013(10) -0.005(9) C20 0.058(8) 0.081(10) 0.109(12) -0.029(9) 0.024(8) 0.007(8) C21 0.047(7) 0.060(7) 0.069(7) -0.007(7) 0.024(7) 0.006(6) C22 0.053(8) 0.089(10) 0.131(12) 0.002(9) 0.001(9) -0.013(7) C23 0.039(7) 0.074(8) 0.047(7) 0.014(6) 0.003(6) -0.007(7) C24 0.085(9) 0.063(8) 0.064(7) 0.023(6) 0.023(8) 0.012(8) C25 0.101(11) 0.101(11) 0.102(12) 0.028(9) -0.004(11) -0.004(11) C26 0.101(12) 0.123(14) 0.114(14) 0.068(11) -0.007(11) -0.003(11) C27 0.092(11) 0.081(9) 0.115(12) 0.052(9) -0.017(10) 0.017(10) C28 0.056(8) 0.095(10) 0.090(10) 0.005(9) 0.010(8) 0.011(8) C29 0.049(7) 0.044(7) 0.069(8) -0.001(6) 0.015(6) 0.012(6) C30 0.063(8) 0.062(7) 0.073(8) -0.012(7) 0.009(7) -0.013(7) C31 0.065(8) 0.061(7) 0.103(9) -0.017(9) 0.023(8) 0.003(8) C32 0.069(8) 0.072(9) 0.087(10) -0.038(8) 0.016(8) -0.001(8) C33 0.086(10) 0.104(11) 0.051(8) -0.020(8) 0.028(8) 0.005(9) C34 0.064(8) 0.063(8) 0.070(9) -0.009(7) 0.018(7) 0.007(7) C35 0.045(7) 0.042(7) 0.055(6) -0.010(5) -0.011(5) 0.008(5) C36 0.110(11) 0.095(10) 0.072(8) 0.019(7) -0.017(7) -0.014(9) C37 0.111(13) 0.190(19) 0.174(16) -0.004(15) 0.059(12) -0.055(14) O1 0.083(6) 0.118(7) 0.082(5) 0.017(5) 0.024(5) -0.012(6) P3 0.104(3) 0.063(3) 0.063(2) 0.005(2) 0.010(2) 0.001(2) F1 0.308(19) 0.37(2) 0.124(9) 0.058(12) 0.050(11) -0.100(17) F2 0.51(3) 0.100(8) 0.242(15) -0.062(9) -0.185(17) 0.068(12) F3 0.185(13) 0.58(3) 0.169(12) 0.157(16) 0.086(10) -0.012(19) F4 0.54(3) 0.069(7) 0.34(2) -0.071(10) -0.13(2) 0.028(12) F5 0.172(11) 0.295(17) 0.291(15) 0.144(15) -0.071(12) 0.016(11) F6 0.135(10) 0.271(16) 0.332(18) 0.113(14) -0.129(12) -0.015(10) _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 C35 1.921(10) . ? Ru1 C3 2.232(11) . ? Ru1 C2 2.256(11) . ? Ru1 C4 2.258(9) . ? Ru1 C5 2.269(11) . ? Ru1 C1 2.294(13) . ? Ru1 P2 2.311(3) . ? Ru1 P1 2.314(3) . ? P1 C7 1.808(10) . ? P1 C15 1.824(11) . ? P1 C9 1.828(11) . ? P2 C21 1.804(10) . ? P2 C23 1.831(10) . ? P2 C29 1.832(11) . ? C1 C5 1.364(16) . ? C1 C2 1.449(16) . ? C1 C6 1.519(17) . ? C2 C3 1.394(15) . ? C3 C4 1.405(15) . ? C4 C5 1.411(14) . ? C7 C8 1.341(14) . ? C9 C10 1.378(14) . ? C9 C14 1.385(13) . ? C10 C11 1.379(16) . ? C11 C12 1.389(18) . ? C12 C13 1.362(16) . ? C13 C14 1.388(15) . ? C15 C16 1.385(14) . ? C15 C20 1.400(15) . ? C16 C17 1.384(14) . ? C17 C18 1.334(17) . ? C18 C19 1.378(18) . ? C19 C20 1.388(17) . ? C21 C22 1.252(13) . ? C23 C28 1.361(14) . ? C23 C24 1.370(14) . ? C24 C25 1.388(15) . ? C25 C26 1.369(18) . ? C26 C27 1.346(18) . ? C27 C28 1.391(14) . ? C29 C30 1.381(13) . ? C29 C34 1.386(13) . ? C30 C31 1.387(13) . ? C31 C32 1.359(15) . ? C32 C33 1.337(15) . ? C33 C34 1.387(14) . ? C35 O1 1.288(11) . ? C35 C36 1.525(11) . ? C37 O1 1.508(14) . ? P3 F4 1.372(10) . ? P3 F3 1.409(10) . ? P3 F2 1.441(11) . ? P3 F6 1.457(10) . ? P3 F1 1.477(11) . ? P3 F5 1.520(12) . ? 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 C35 Ru1 C3 119.2(4) . . ? C35 Ru1 C2 94.7(4) . . ? C3 Ru1 C2 36.2(4) . . ? C35 Ru1 C4 154.2(4) . . ? C3 Ru1 C4 36.5(4) . . ? C2 Ru1 C4 60.2(4) . . ? C35 Ru1 C5 137.4(4) . . ? C3 Ru1 C5 60.5(4) . . ? C2 Ru1 C5 59.8(4) . . ? C4 Ru1 C5 36.3(4) . . ? C35 Ru1 C1 104.2(5) . . ? C3 Ru1 C1 61.1(4) . . ? C2 Ru1 C1 37.1(4) . . ? C4 Ru1 C1 60.0(4) . . ? C5 Ru1 C1 34.8(4) . . ? C35 Ru1 P2 88.2(3) . . ? C3 Ru1 P2 151.0(3) . . ? C2 Ru1 P2 141.9(4) . . ? C4 Ru1 P2 114.8(4) . . ? C5 Ru1 P2 93.4(3) . . ? C1 Ru1 P2 105.5(4) . . ? C35 Ru1 P1 92.8(3) . . ? C3 Ru1 P1 91.4(3) . . ? C2 Ru1 P1 120.8(4) . . ? C4 Ru1 P1 95.7(3) . . ? C5 Ru1 P1 129.1(3) . . ? C1 Ru1 P1 152.1(3) . . ? P2 Ru1 P1 96.86(11) . . ? C7 P1 C15 103.4(5) . . ? C7 P1 C9 102.1(5) . . ? C15 P1 C9 103.4(5) . . ? C7 P1 Ru1 108.7(4) . . ? C15 P1 Ru1 115.6(4) . . ? C9 P1 Ru1 121.5(4) . . ? C21 P2 C23 101.6(5) . . ? C21 P2 C29 105.0(5) . . ? C23 P2 C29 102.2(5) . . ? C21 P2 Ru1 117.5(4) . . ? C23 P2 Ru1 118.0(4) . . ? C29 P2 Ru1 110.8(4) . . ? C5 C1 C2 106.5(12) . . ? C5 C1 C6 126.4(14) . . ? C2 C1 C6 125.8(14) . . ? C5 C1 Ru1 71.6(7) . . ? C2 C1 Ru1 70.0(7) . . ? C6 C1 Ru1 133.3(9) . . ? C3 C2 C1 108.1(12) . . ? C3 C2 Ru1 71.0(7) . . ? C1 C2 Ru1 72.9(7) . . ? C2 C3 C4 107.9(12) . . ? C2 C3 Ru1 72.8(7) . . ? C4 C3 Ru1 72.8(6) . . ? C3 C4 C5 107.3(10) . . ? C3 C4 Ru1 70.8(6) . . ? C5 C4 Ru1 72.3(6) . . ? C1 C5 C4 110.2(11) . . ? C1 C5 Ru1 73.6(8) . . ? C4 C5 Ru1 71.4(6) . . ? C8 C7 P1 125.7(10) . . ? C10 C9 C14 117.8(11) . . ? C10 C9 P1 121.6(9) . . ? C14 C9 P1 120.3(9) . . ? C9 C10 C11 121.0(12) . . ? C10 C11 C12 119.8(14) . . ? C13 C12 C11 120.6(13) . . ? C12 C13 C14 118.6(13) . . ? C9 C14 C13 122.2(12) . . ? C16 C15 C20 118.3(11) . . ? C16 C15 P1 122.8(9) . . ? C20 C15 P1 118.9(10) . . ? C17 C16 C15 120.4(11) . . ? C18 C17 C16 120.7(14) . . ? C17 C18 C19 120.9(14) . . ? C18 C19 C20 119.7(14) . . ? C19 C20 C15 119.9(14) . . ? C22 C21 P2 128.4(10) . . ? C28 C23 C24 116.6(10) . . ? C28 C23 P2 122.4(9) . . ? C24 C23 P2 120.9(9) . . ? C23 C24 C25 121.9(12) . . ? C26 C25 C24 118.8(15) . . ? C27 C26 C25 121.2(14) . . ? C26 C27 C28 118.3(13) . . ? C23 C28 C27 123.1(12) . . ? C30 C29 C34 117.2(11) . . ? C30 C29 P2 122.5(9) . . ? C34 C29 P2 120.1(9) . . ? C29 C30 C31 123.6(11) . . ? C32 C31 C30 115.5(12) . . ? C33 C32 C31 124.3(12) . . ? C32 C33 C34 119.3(12) . . ? C29 C34 C33 120.1(11) . . ? O1 C35 C36 113.0(9) . . ? O1 C35 Ru1 122.0(7) . . ? C36 C35 Ru1 125.0(8) . . ? C35 O1 C37 121.4(10) . . ? F4 P3 F3 87.9(11) . . ? F4 P3 F2 172.2(13) . . ? F3 P3 F2 96.9(12) . . ? F4 P3 F6 94.3(10) . . ? F3 P3 F6 93.2(8) . . ? F2 P3 F6 91.5(8) . . ? F4 P3 F1 93.7(11) . . ? F3 P3 F1 178.4(12) . . ? F2 P3 F1 81.6(9) . . ? F6 P3 F1 86.1(8) . . ? F4 P3 F5 89.9(10) . . ? F3 P3 F5 86.7(8) . . ? F2 P3 F5 84.3(9) . . ? F6 P3 F5 175.8(10) . . ? F1 P3 F5 93.8(9) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 22.51 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.549 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.067 #===END data_jhn447b _database_code_CSD 195529 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 8 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H35 Cl2 F6 O P3 Ru' _chemical_formula_weight 862.52 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' O O 0.0106 0.0060 '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' Ru Ru -1.2594 0.8363 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.464(2) _cell_length_b 10.951(4) _cell_length_c 18.964(7) _cell_angle_alpha 90.68(4) _cell_angle_beta 103.09(3) _cell_angle_gamma 101.30(3) _cell_volume 1874.1(11) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 3.68 _cell_measurement_theta_max 12.15 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max .24 _exptl_crystal_size_mid .40 _exptl_crystal_size_min .32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.747 _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 298(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7019 _diffrn_reflns_av_R_equivalents 0.1644 _diffrn_reflns_av_sigmaI/netI 0.2152 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5851 _reflns_number_gt 2815 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1300P)^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_number_reflns 5851 _refine_ls_number_parameters 442 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.2121 _refine_ls_R_factor_gt 0.1040 _refine_ls_wR_factor_ref 0.2904 _refine_ls_wR_factor_gt 0.2298 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.030 _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 Ru1 Ru 0.95097(13) -0.23998(11) 0.74106(6) 0.0426(4) Uani 1 1 d . . . P1 P 0.7185(4) -0.2006(3) 0.6870(2) 0.0470(10) Uani 1 1 d . . . P2 P 0.9489(4) -0.1776(3) 0.85812(19) 0.0429(9) Uani 1 1 d . . . C1 C 1.0714(19) -0.1363(19) 0.6594(9) 0.073(5) Uani 1 1 d . . . C2 C 1.1414(16) -0.0884(16) 0.7291(9) 0.064(4) Uani 1 1 d . . . H2A H 1.1599 -0.0009 0.7468 0.076 Uiso 1 1 calc R . . C3 C 1.1935(16) -0.1878(18) 0.7690(10) 0.070(5) Uani 1 1 d . . . H3A H 1.2575 -0.1795 0.8180 0.084 Uiso 1 1 calc R . . C4 C 1.1536(19) -0.2946(17) 0.7217(12) 0.083(6) Uani 1 1 d . . . H4A H 1.1827 -0.3746 0.7329 0.099 Uiso 1 1 calc R . . C5 C 1.0742(19) -0.2661(16) 0.6546(10) 0.069(5) Uani 1 1 d . . . H5A H 1.0366 -0.3224 0.6110 0.082 Uiso 1 1 calc R . . C6 C 1.027(3) -0.056(3) 0.6009(12) 0.145(10) Uani 1 1 d . . . H6A H 1.1076 -0.0287 0.5783 0.218 Uiso 1 1 calc R . . H6B H 0.9996 0.0149 0.6203 0.218 Uiso 1 1 calc R . . H6C H 0.9434 -0.1022 0.5655 0.218 Uiso 1 1 calc R . . C7 C 0.5661(17) -0.3077(14) 0.7085(9) 0.062(4) Uani 1 1 d . . . H7A H 0.5636 -0.3131 0.7571 0.074 Uiso 1 1 calc R . . C8 C 0.459(2) -0.3781(16) 0.6612(12) 0.099(7) Uani 1 1 d . . . H8A H 0.4580 -0.3753 0.6121 0.118 Uiso 1 1 calc R . . H8B H 0.3841 -0.4313 0.6765 0.118 Uiso 1 1 calc R . . C9 C 0.6777(16) -0.2181(14) 0.5864(7) 0.055(4) Uani 1 1 d . . . C10 C 0.6941(19) -0.3272(16) 0.5573(9) 0.079(5) Uani 1 1 d . . . H10A H 0.7191 -0.3908 0.5866 0.094 Uiso 1 1 calc R . . C11 C 0.672(2) -0.340(2) 0.4816(11) 0.094(6) Uani 1 1 d . . . H11A H 0.6881 -0.4122 0.4606 0.113 Uiso 1 1 calc R . . C12 C 0.628(2) -0.251(3) 0.4388(10) 0.114(8) Uani 1 1 d . . . H12A H 0.6086 -0.2635 0.3886 0.137 Uiso 1 1 calc R . . C13 C 0.613(3) -0.148(2) 0.4680(11) 0.114(8) Uani 1 1 d . . . H13A H 0.5880 -0.0846 0.4382 0.137 Uiso 1 1 calc R . . C14 C 0.633(2) -0.1288(19) 0.5436(8) 0.086(6) Uani 1 1 d . . . H14A H 0.6152 -0.0567 0.5635 0.104 Uiso 1 1 calc R . . C15 C 0.6796(15) -0.0492(13) 0.7061(7) 0.048(4) Uani 1 1 d . . . C16 C 0.5389(15) -0.0335(14) 0.7093(7) 0.054(4) Uani 1 1 d . . . H16A H 0.4601 -0.1017 0.6999 0.065 Uiso 1 1 calc R . . C17 C 0.5155(17) 0.0820(15) 0.7265(8) 0.064(4) Uani 1 1 d . . . H17A H 0.4209 0.0908 0.7288 0.077 Uiso 1 1 calc R . . C18 C 0.631(2) 0.1860(15) 0.7403(9) 0.076(5) Uani 1 1 d . . . H18A H 0.6162 0.2632 0.7547 0.092 Uiso 1 1 calc R . . C19 C 0.7705(16) 0.1707(13) 0.7320(7) 0.052(4) Uani 1 1 d . . . H19A H 0.8469 0.2402 0.7363 0.062 Uiso 1 1 calc R . . C20 C 0.7950(16) 0.0573(13) 0.7179(7) 0.052(4) Uani 1 1 d . . . H20A H 0.8899 0.0488 0.7159 0.062 Uiso 1 1 calc R . . C21 C 1.0510(16) -0.0180(12) 0.8791(8) 0.054(4) Uani 1 1 d . . . H21A H 1.0054 0.0440 0.8568 0.065 Uiso 1 1 calc R . . C22 C 1.1795(17) 0.0180(16) 0.9215(8) 0.075(5) Uani 1 1 d . . . H22A H 1.2297 -0.0404 0.9451 0.090 Uiso 1 1 calc R . . H22B H 1.2225 0.1025 0.9287 0.090 Uiso 1 1 calc R . . C23 C 0.7742(15) -0.1783(13) 0.8846(7) 0.045(4) Uani 1 1 d . . . C24 C 0.7025(16) -0.2915(14) 0.9074(9) 0.064(4) Uani 1 1 d . . . H24A H 0.7430 -0.3625 0.9092 0.077 Uiso 1 1 calc R . . C25 C 0.568(2) -0.293(2) 0.9272(10) 0.093(6) Uani 1 1 d . . . H25A H 0.5159 -0.3674 0.9396 0.112 Uiso 1 1 calc R . . C26 C 0.5139(19) -0.188(2) 0.9287(9) 0.077(5) Uani 1 1 d . . . H26A H 0.4275 -0.1917 0.9448 0.092 Uiso 1 1 calc R . . C27 C 0.5794(18) -0.0795(17) 0.9078(9) 0.068(5) Uani 1 1 d . . . H27A H 0.5369 -0.0097 0.9076 0.081 Uiso 1 1 calc R . . C28 C 0.7143(16) -0.0722(15) 0.8860(7) 0.056(4) Uani 1 1 d . . . H28A H 0.7627 0.0033 0.8726 0.067 Uiso 1 1 calc R . . C29 C 1.0443(15) -0.2647(11) 0.9305(7) 0.043(3) Uani 1 1 d . . . C30 C 1.1119(15) -0.3583(13) 0.9175(8) 0.049(4) Uani 1 1 d . . . H30A H 1.1087 -0.3838 0.8701 0.059 Uiso 1 1 calc R . . C31 C 1.1840(17) -0.4144(14) 0.9738(10) 0.065(4) Uani 1 1 d . . . H31A H 1.2256 -0.4810 0.9640 0.078 Uiso 1 1 calc R . . C32 C 1.198(2) -0.3779(16) 1.0431(10) 0.079(5) Uani 1 1 d . . . H32A H 1.2559 -0.4130 1.0806 0.095 Uiso 1 1 calc R . . C33 C 1.126(2) -0.2893(15) 1.0573(8) 0.073(5) Uani 1 1 d . . . H33A H 1.1297 -0.2660 1.1051 0.088 Uiso 1 1 calc R . . C34 C 1.049(2) -0.2338(16) 1.0024(9) 0.077(5) Uani 1 1 d . . . H34A H 0.9984 -0.1739 1.0129 0.092 Uiso 1 1 calc R . . C35 C 0.8595(18) -0.4039(18) 0.7524(9) 0.072(5) Uani 1 1 d . . . O1 O 0.8054(13) -0.5060(10) 0.7625(7) 0.089(4) Uani 1 1 d . . . P3 P 1.2556(8) 0.3392(5) 0.7936(4) 0.0991(19) Uani 1 1 d . . . F1 F 1.184(4) 0.313(2) 0.8518(15) 0.319(17) Uani 1 1 d . . . F2 F 1.135(3) 0.4013(16) 0.7512(17) 0.335(19) Uani 1 1 d . . . F3 F 1.165(2) 0.2150(14) 0.7554(13) 0.228(9) Uani 1 1 d . . . F4 F 1.365(2) 0.258(3) 0.8323(12) 0.251(11) Uani 1 1 d . . . F5 F 1.338(3) 0.3473(19) 0.7368(14) 0.288(14) Uani 1 1 d . . . F6 F 1.320(3) 0.4714(16) 0.8178(11) 0.239(10) Uani 1 1 d . . . Cl1 Cl 0.826(7) 0.212(3) 0.530(3) 0.80(4) Uani 1 1 d . . . Cl2 Cl 0.943(4) 0.411(3) 0.559(2) 0.69(4) Uani 1 1 d . . . C36 C 0.753(7) 0.317(8) 0.551(4) 0.41(4) Uani 1 1 d U . . H36A H 0.7225 0.3087 0.5968 0.494 Uiso 1 1 calc R . . H36B H 0.6772 0.3389 0.5128 0.494 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0424(7) 0.0402(7) 0.0446(7) -0.0019(5) 0.0085(5) 0.0090(5) P1 0.047(2) 0.043(2) 0.048(2) -0.0044(17) 0.0062(18) 0.0067(18) P2 0.045(2) 0.038(2) 0.043(2) -0.0010(16) 0.0056(18) 0.0085(17) C1 0.065(11) 0.114(16) 0.049(10) 0.024(10) 0.027(9) 0.018(11) C2 0.043(9) 0.068(11) 0.085(13) -0.003(10) 0.035(9) 0.000(8) C3 0.037(9) 0.091(14) 0.085(13) 0.012(11) 0.022(9) 0.013(9) C4 0.064(12) 0.070(13) 0.146(19) 0.033(13) 0.065(13) 0.038(10) C5 0.080(13) 0.059(11) 0.073(12) -0.012(9) 0.027(10) 0.020(10) C6 0.11(2) 0.22(3) 0.110(19) 0.03(2) 0.042(16) 0.04(2) C7 0.050(10) 0.060(10) 0.069(11) -0.008(8) 0.009(8) 0.003(8) C8 0.074(14) 0.075(13) 0.144(19) -0.010(13) 0.050(13) -0.019(11) C9 0.058(10) 0.065(10) 0.040(9) -0.005(8) 0.003(7) 0.015(8) C10 0.088(13) 0.069(11) 0.072(12) -0.027(9) 0.001(10) 0.021(10) C11 0.115(17) 0.109(16) 0.067(13) -0.021(12) 0.014(12) 0.054(14) C12 0.124(19) 0.18(3) 0.044(12) -0.020(14) -0.001(11) 0.076(18) C13 0.16(2) 0.130(19) 0.064(13) 0.016(13) 0.011(14) 0.078(17) C14 0.109(15) 0.128(17) 0.034(9) 0.017(10) 0.004(10) 0.067(13) C15 0.047(9) 0.050(9) 0.052(9) 0.003(7) 0.009(7) 0.028(7) C16 0.041(9) 0.066(10) 0.050(9) 0.003(7) 0.008(7) 0.005(8) C17 0.042(9) 0.062(11) 0.082(12) -0.018(9) -0.008(8) 0.019(8) C18 0.084(14) 0.058(11) 0.075(12) -0.018(9) -0.014(10) 0.024(10) C19 0.050(10) 0.048(9) 0.052(9) 0.008(7) 0.005(7) 0.007(8) C20 0.052(9) 0.049(9) 0.056(9) -0.009(7) 0.026(8) 0.001(8) C21 0.052(10) 0.038(8) 0.074(11) 0.005(7) 0.013(8) 0.016(7) C22 0.057(11) 0.075(12) 0.074(12) -0.016(9) -0.021(9) 0.012(9) C23 0.044(8) 0.050(9) 0.034(8) -0.016(6) -0.012(6) 0.014(7) C24 0.040(9) 0.051(10) 0.105(13) 0.018(9) 0.027(9) 0.002(8) C25 0.084(15) 0.091(16) 0.093(15) 0.010(12) 0.020(12) -0.009(12) C26 0.048(11) 0.095(15) 0.082(13) -0.012(11) 0.008(9) 0.013(11) C27 0.067(12) 0.072(12) 0.072(11) -0.010(9) 0.019(9) 0.030(10) C28 0.063(10) 0.072(11) 0.038(8) 0.004(7) 0.011(7) 0.026(9) C29 0.050(9) 0.024(7) 0.051(9) -0.002(6) 0.004(7) 0.009(6) C30 0.057(9) 0.049(9) 0.044(8) 0.013(7) 0.017(7) 0.010(8) C31 0.054(10) 0.053(10) 0.088(13) 0.008(10) 0.014(10) 0.011(8) C32 0.092(14) 0.066(12) 0.067(13) 0.017(10) -0.007(11) 0.015(11) C33 0.133(16) 0.064(11) 0.031(8) 0.019(8) 0.015(10) 0.043(11) C34 0.098(14) 0.073(12) 0.060(11) -0.021(9) 0.008(10) 0.031(10) C35 0.054(11) 0.082(14) 0.071(12) -0.003(10) -0.004(9) 0.013(10) O1 0.083(9) 0.040(7) 0.137(12) -0.006(7) 0.027(8) -0.009(6) P3 0.116(5) 0.061(3) 0.137(5) -0.005(3) 0.067(5) 0.015(3) F1 0.57(5) 0.22(2) 0.35(3) 0.13(2) 0.38(3) 0.20(3) F2 0.26(2) 0.101(13) 0.55(4) 0.003(19) -0.15(3) 0.087(15) F3 0.205(19) 0.080(10) 0.38(3) 0.015(14) 0.069(19) -0.016(11) F4 0.175(18) 0.37(3) 0.25(2) 0.13(2) 0.081(17) 0.12(2) F5 0.45(4) 0.20(2) 0.33(3) 0.042(19) 0.31(3) 0.09(2) F6 0.33(3) 0.118(13) 0.23(2) -0.084(13) 0.083(18) -0.059(15) Cl1 1.37(12) 0.48(5) 0.78(7) 0.23(5) 0.72(8) 0.20(6) Cl2 0.52(5) 0.47(5) 1.00(10) -0.33(5) -0.06(5) 0.17(5) C36 0.22(5) 0.59(10) 0.35(7) 0.18(7) 0.01(5) -0.03(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 Ru1 C35 1.87(2) . ? Ru1 C3 2.192(15) . ? Ru1 C4 2.221(15) . ? Ru1 C2 2.253(15) . ? Ru1 C5 2.261(15) . ? Ru1 C1 2.307(16) . ? Ru1 P2 2.320(4) . ? Ru1 P1 2.332(4) . ? P1 C7 1.799(16) . ? P1 C15 1.817(13) . ? P1 C9 1.859(14) . ? P2 C21 1.815(14) . ? P2 C23 1.833(14) . ? P2 C29 1.848(13) . ? C1 C2 1.38(2) . ? C1 C5 1.43(2) . ? C1 C6 1.46(3) . ? C2 C3 1.44(2) . ? C3 C4 1.40(2) . ? C4 C5 1.40(2) . ? C7 C8 1.30(2) . ? C9 C14 1.35(2) . ? C9 C10 1.36(2) . ? C10 C11 1.40(2) . ? C11 C12 1.34(3) . ? C12 C13 1.30(3) . ? C13 C14 1.41(2) . ? C15 C16 1.391(18) . ? C15 C20 1.409(18) . ? C16 C17 1.374(19) . ? C17 C18 1.39(2) . ? C18 C19 1.41(2) . ? C19 C20 1.342(18) . ? C21 C22 1.282(18) . ? C23 C28 1.392(18) . ? C23 C24 1.414(19) . ? C24 C25 1.40(2) . ? C25 C26 1.35(2) . ? C26 C27 1.34(2) . ? C27 C28 1.42(2) . ? C29 C30 1.357(18) . ? C29 C34 1.390(19) . ? C30 C31 1.354(19) . ? C31 C32 1.34(2) . ? C32 C33 1.35(2) . ? C33 C34 1.35(2) . ? C35 O1 1.172(19) . ? P3 F1 1.427(17) . ? P3 F5 1.458(17) . ? P3 F6 1.480(15) . ? P3 F2 1.522(18) . ? P3 F3 1.533(17) . ? P3 F4 1.56(2) . ? Cl1 C36 1.55(9) . ? Cl1 Cl2 2.24(5) . ? Cl2 C36 1.86(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 C35 Ru1 C3 119.1(7) . . ? C35 Ru1 C4 93.6(7) . . ? C3 Ru1 C4 37.0(6) . . ? C35 Ru1 C2 154.8(7) . . ? C3 Ru1 C2 37.7(6) . . ? C4 Ru1 C2 61.5(6) . . ? C35 Ru1 C5 102.3(7) . . ? C3 Ru1 C5 61.4(6) . . ? C4 Ru1 C5 36.3(6) . . ? C2 Ru1 C5 60.9(6) . . ? C35 Ru1 C1 137.1(7) . . ? C3 Ru1 C1 60.6(6) . . ? C4 Ru1 C1 60.2(7) . . ? C2 Ru1 C1 35.3(6) . . ? C5 Ru1 C1 36.5(6) . . ? C35 Ru1 P2 91.9(5) . . ? C3 Ru1 P2 89.5(5) . . ? C4 Ru1 P2 118.6(6) . . ? C2 Ru1 P2 96.4(4) . . ? C5 Ru1 P2 150.9(5) . . ? C1 Ru1 P2 129.8(5) . . ? C35 Ru1 P1 88.8(5) . . ? C3 Ru1 P1 151.5(5) . . ? C4 Ru1 P1 145.4(6) . . ? C2 Ru1 P1 113.9(5) . . ? C5 Ru1 P1 109.6(5) . . ? C1 Ru1 P1 95.6(5) . . ? P2 Ru1 P1 95.76(13) . . ? C7 P1 C15 103.0(7) . . ? C7 P1 C9 103.0(7) . . ? C15 P1 C9 104.4(7) . . ? C7 P1 Ru1 114.2(5) . . ? C15 P1 Ru1 118.4(5) . . ? C9 P1 Ru1 112.2(5) . . ? C21 P2 C23 104.2(6) . . ? C21 P2 C29 103.5(6) . . ? C23 P2 C29 101.7(6) . . ? C21 P2 Ru1 109.5(5) . . ? C23 P2 Ru1 121.0(4) . . ? C29 P2 Ru1 115.1(4) . . ? C2 C1 C5 108.9(16) . . ? C2 C1 C6 122(2) . . ? C5 C1 C6 128.4(19) . . ? C2 C1 Ru1 70.3(9) . . ? C5 C1 Ru1 70.1(9) . . ? C6 C1 Ru1 133.0(14) . . ? C1 C2 C3 107.5(16) . . ? C1 C2 Ru1 74.5(9) . . ? C3 C2 Ru1 68.9(9) . . ? C4 C3 C2 107.5(16) . . ? C4 C3 Ru1 72.6(9) . . ? C2 C3 Ru1 73.5(9) . . ? C5 C4 C3 108.9(16) . . ? C5 C4 Ru1 73.4(9) . . ? C3 C4 Ru1 70.4(9) . . ? C4 C5 C1 107.1(15) . . ? C4 C5 Ru1 70.3(9) . . ? C1 C5 Ru1 73.5(9) . . ? C8 C7 P1 125.0(15) . . ? C14 C9 C10 121.0(15) . . ? C14 C9 P1 122.5(12) . . ? C10 C9 P1 116.5(13) . . ? C9 C10 C11 117.8(18) . . ? C12 C11 C10 121.2(18) . . ? C13 C12 C11 119.7(18) . . ? C12 C13 C14 122(2) . . ? C9 C14 C13 118.2(17) . . ? C16 C15 C20 118.0(13) . . ? C16 C15 P1 122.4(11) . . ? C20 C15 P1 119.5(10) . . ? C17 C16 C15 120.5(14) . . ? C16 C17 C18 121.1(15) . . ? C17 C18 C19 117.9(14) . . ? C20 C19 C18 121.0(14) . . ? C19 C20 C15 121.2(14) . . ? C22 C21 P2 126.6(13) . . ? C28 C23 C24 119.7(14) . . ? C28 C23 P2 122.9(12) . . ? C24 C23 P2 117.4(10) . . ? C25 C24 C23 117.7(15) . . ? C26 C25 C24 121.1(18) . . ? C27 C26 C25 122.6(18) . . ? C26 C27 C28 119.0(16) . . ? C23 C28 C27 119.8(15) . . ? C30 C29 C34 117.2(13) . . ? C30 C29 P2 123.5(10) . . ? C34 C29 P2 119.3(11) . . ? C31 C30 C29 119.8(14) . . ? C32 C31 C30 122.8(16) . . ? C31 C32 C33 118.4(16) . . ? C32 C33 C34 120.3(15) . . ? C33 C34 C29 121.2(15) . . ? O1 C35 Ru1 177.2(15) . . ? F1 P3 F5 170.5(13) . . ? F1 P3 F6 95.5(14) . . ? F5 P3 F6 91.0(12) . . ? F1 P3 F2 93.5(18) . . ? F5 P3 F2 94.5(18) . . ? F6 P3 F2 79.8(12) . . ? F1 P3 F3 88.1(14) . . ? F5 P3 F3 87.1(13) . . ? F6 P3 F3 166.9(14) . . ? F2 P3 F3 87.5(11) . . ? F1 P3 F4 85.4(13) . . ? F5 P3 F4 86.0(13) . . ? F6 P3 F4 108.3(15) . . ? F2 P3 F4 172.0(13) . . ? F3 P3 F4 84.5(12) . . ? C36 Cl1 Cl2 55(3) . . ? C36 Cl2 Cl1 43(3) . . ? Cl1 C36 Cl2 82(4) . . ? _diffrn_measured_fraction_theta_max 0.746 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.746 _refine_diff_density_max 0.868 _refine_diff_density_min -0.952 _refine_diff_density_rms 0.136 #===END data_jhn353b _database_code_CSD 195530 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 11 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H7 O2 Ru' _chemical_formula_weight 236.21 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' O O 0.0106 0.0060 '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 P2(1)/c 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 8.0001(12) _cell_length_b 11.9948(14) _cell_length_c 8.2434(14) _cell_angle_alpha 90.00 _cell_angle_beta 100.329(16) _cell_angle_gamma 90.00 _cell_volume 778.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.02 _cell_measurement_theta_max 12.51 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max .14 _exptl_crystal_size_mid .44 _exptl_crystal_size_min .42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 1.954 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5074 _exptl_absorpt_correction_T_max 0.9990 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2958 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 30.00 _reflns_number_total 2279 _reflns_number_gt 1981 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0562P)^2^+0.1102P] 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_coef 0.0140(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2279 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.63672(2) 0.510028(17) 0.12598(2) 0.02870(10) Uani 1 1 d . . . C1 C 0.8449(4) 0.3745(3) 0.1976(3) 0.0422(6) Uani 1 1 d . . . C2 C 0.8874(4) 0.4744(3) 0.2852(4) 0.0432(6) Uani 1 1 d . . . H2A H 0.9916 0.5173 0.2847 0.052 Uiso 1 1 calc R . . C3 C 0.7685(5) 0.4959(3) 0.3892(4) 0.0491(8) Uani 1 1 d . . . H3A H 0.7771 0.5548 0.4727 0.059 Uiso 1 1 calc R . . C4 C 0.6463(5) 0.4114(3) 0.3638(4) 0.0532(8) Uani 1 1 d . . . H4A H 0.5525 0.4016 0.4244 0.064 Uiso 1 1 calc R . . C5 C 0.6891(4) 0.3385(3) 0.2422(4) 0.0484(7) Uani 1 1 d . . . H5A H 0.6280 0.2700 0.2035 0.058 Uiso 1 1 calc R . . C6 C 0.9448(5) 0.3157(4) 0.0874(5) 0.0689(12) Uani 1 1 d . . . H6A H 1.0217 0.2641 0.1511 0.103 Uiso 1 1 calc R . . H6B H 1.0081 0.3692 0.0364 0.103 Uiso 1 1 calc R . . H6C H 0.8688 0.2759 0.0038 0.103 Uiso 1 1 calc R . . C7 C 0.6629(4) 0.6611(3) 0.0882(4) 0.0423(6) Uani 1 1 d . . . C8 C 0.3795(3) 0.5272(2) 0.1171(3) 0.0330(5) Uani 1 1 d . . . O1 O 0.6847(4) 0.7542(2) 0.0694(4) 0.0727(8) Uani 1 1 d . . . O2 O 0.2897(3) 0.5489(2) 0.2101(2) 0.0505(5) Uani 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 Ru1 0.02278(13) 0.03235(14) 0.02887(14) 0.00090(7) -0.00102(8) 0.00002(7) C1 0.0346(14) 0.0487(16) 0.0387(13) 0.0000(11) -0.0056(11) 0.0128(12) C2 0.0297(14) 0.0536(16) 0.0405(14) 0.0009(12) -0.0094(11) -0.0021(12) C3 0.049(2) 0.062(2) 0.0297(13) -0.0048(11) -0.0108(13) 0.0133(14) C4 0.0463(18) 0.072(2) 0.0409(15) 0.0211(15) 0.0077(13) 0.0130(16) C5 0.0439(17) 0.0387(15) 0.0565(17) 0.0158(13) -0.0075(14) -0.0005(12) C6 0.059(2) 0.085(3) 0.059(2) -0.0120(19) -0.0006(17) 0.037(2) C7 0.0297(14) 0.0406(15) 0.0548(16) -0.0008(12) 0.0028(12) -0.0004(11) C8 0.0247(12) 0.0390(13) 0.0334(12) 0.0026(10) 0.0005(9) 0.0033(10) O1 0.0659(17) 0.0375(12) 0.114(2) 0.0078(14) 0.0133(17) -0.0051(12) O2 0.0363(11) 0.0762(16) 0.0403(11) -0.0021(10) 0.0106(9) 0.0075(11) _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 C7 1.857(3) . ? Ru1 C8 2.034(3) 3_665 ? Ru1 C8 2.056(3) . ? Ru1 C2 2.233(3) . ? Ru1 C3 2.242(3) . ? Ru1 C5 2.277(3) . ? Ru1 C4 2.279(3) . ? Ru1 C1 2.327(3) . ? Ru1 Ru1 2.7437(7) 3_665 ? C1 C2 1.409(4) . ? C1 C5 1.428(5) . ? C1 C6 1.490(4) . ? C2 C3 1.414(5) . ? C3 C4 1.398(5) . ? C4 C5 1.418(5) . ? C7 O1 1.145(4) . ? C8 O2 1.170(3) . ? C8 Ru1 2.034(3) 3_665 ? 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 C7 Ru1 C8 92.21(12) . 3_665 ? C7 Ru1 C8 92.19(12) . . ? C8 Ru1 C8 95.74(10) 3_665 . ? C7 Ru1 C2 99.74(12) . . ? C8 Ru1 C2 115.41(12) 3_665 . ? C8 Ru1 C2 145.89(12) . . ? C7 Ru1 C3 100.85(13) . . ? C8 Ru1 C3 150.76(12) 3_665 . ? C8 Ru1 C3 109.63(13) . . ? C2 Ru1 C3 36.84(14) . . ? C7 Ru1 C5 159.19(12) . . ? C8 Ru1 C5 100.97(12) 3_665 . ? C8 Ru1 C5 102.32(11) . . ? C2 Ru1 C5 60.08(12) . . ? C3 Ru1 C5 60.36(12) . . ? C7 Ru1 C4 131.55(14) . . ? C8 Ru1 C4 136.02(13) 3_665 . ? C8 Ru1 C4 87.81(12) . . ? C2 Ru1 C4 60.45(13) . . ? C3 Ru1 C4 36.01(14) . . ? C5 Ru1 C4 36.27(13) . . ? C7 Ru1 C1 128.87(12) . . ? C8 Ru1 C1 90.74(10) 3_665 . ? C8 Ru1 C1 138.19(11) . . ? C2 Ru1 C1 35.93(11) . . ? C3 Ru1 C1 60.71(11) . . ? C5 Ru1 C1 36.11(12) . . ? C4 Ru1 C1 60.45(12) . . ? C7 Ru1 Ru1 93.28(9) . 3_665 ? C8 Ru1 Ru1 48.21(8) 3_665 3_665 ? C8 Ru1 Ru1 47.53(7) . 3_665 ? C2 Ru1 Ru1 159.82(9) . 3_665 ? C3 Ru1 Ru1 153.98(11) . 3_665 ? C5 Ru1 Ru1 107.52(8) . 3_665 ? C4 Ru1 Ru1 120.32(10) . 3_665 ? C1 Ru1 Ru1 124.62(7) . 3_665 ? C2 C1 C5 105.5(3) . . ? C2 C1 C6 127.5(3) . . ? C5 C1 C6 127.0(3) . . ? C2 C1 Ru1 68.39(17) . . ? C5 C1 Ru1 70.02(16) . . ? C6 C1 Ru1 127.8(2) . . ? C1 C2 C3 109.8(3) . . ? C1 C2 Ru1 75.69(17) . . ? C3 C2 Ru1 71.95(17) . . ? C4 C3 C2 107.8(3) . . ? C4 C3 Ru1 73.44(18) . . ? C2 C3 Ru1 71.22(16) . . ? C3 C4 C5 107.6(3) . . ? C3 C4 Ru1 70.55(18) . . ? C5 C4 Ru1 71.76(17) . . ? C4 C5 C1 109.2(3) . . ? C4 C5 Ru1 71.97(18) . . ? C1 C5 Ru1 73.87(17) . . ? O1 C7 Ru1 177.3(3) . . ? O2 C8 Ru1 139.1(2) . 3_665 ? O2 C8 Ru1 136.7(2) . . ? Ru1 C8 Ru1 84.26(10) 3_665 . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.219 _refine_diff_density_min -1.333 _refine_diff_density_rms 0.119 #===END data_jhn364a _database_code_CSD 195531 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 12 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H7 Br O2 Ru' _chemical_formula_weight 316.12 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.959(5) _cell_length_b 7.662(3) _cell_length_c 9.871(4) _cell_angle_alpha 91.84(3) _cell_angle_beta 93.86(5) _cell_angle_gamma 112.85(4) _cell_volume 483.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.18 _cell_measurement_theta_max 19.55 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max .42 _exptl_crystal_size_mid .46 _exptl_crystal_size_min .44 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 300 _exptl_absorpt_coefficient_mu 5.715 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6002 _exptl_absorpt_correction_T_max 0.9595 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3432 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 30.00 _reflns_number_total 2798 _reflns_number_gt 2128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0680P)^2^+0.1693P] 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_coef 0.050(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2798 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1218 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 Ru1 Ru 0.47414(6) 0.27251(5) 0.27030(4) 0.03804(17) Uani 1 1 d . . . Br1 Br 0.75605(9) 0.60464(8) 0.27656(7) 0.0579(2) Uani 1 1 d . . . C1 C 0.2227(8) 0.3770(8) 0.1878(6) 0.0451(11) Uani 1 1 d . . . C2 C 0.1903(9) 0.3195(9) 0.3227(6) 0.0539(13) Uani 1 1 d . . . H2A H 0.1818 0.3978 0.4007 0.065 Uiso 1 1 calc R . . C3 C 0.1506(9) 0.1224(10) 0.3210(7) 0.0619(16) Uani 1 1 d . . . H3A H 0.1068 0.0409 0.3971 0.074 Uiso 1 1 calc R . . C4 C 0.1697(8) 0.0623(8) 0.1888(7) 0.0580(15) Uani 1 1 d . . . H4A H 0.1407 -0.0686 0.1567 0.070 Uiso 1 1 calc R . . C5 C 0.2152(8) 0.2191(8) 0.1059(6) 0.0489(12) Uani 1 1 d . . . H5A H 0.2287 0.2161 0.0077 0.059 Uiso 1 1 calc R . . C6 C 0.2601(11) 0.5679(9) 0.1384(8) 0.0656(16) Uani 1 1 d . . . H6A H 0.1285 0.5744 0.1098 0.098 Uiso 1 1 calc R . . H6B H 0.3449 0.5893 0.0629 0.098 Uiso 1 1 calc R . . H6C H 0.3311 0.6631 0.2104 0.098 Uiso 1 1 calc R . . C7 C 0.6322(9) 0.1675(9) 0.1733(7) 0.0541(14) Uani 1 1 d . . . O1 O 0.7094(8) 0.0925(8) 0.1100(6) 0.0840(17) Uani 1 1 d . . . C8 C 0.5994(11) 0.2362(9) 0.4360(7) 0.0636(16) Uani 1 1 d . . . O2 O 0.6737(11) 0.2097(8) 0.5344(6) 0.101(2) Uani 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 Ru1 0.0359(2) 0.0336(2) 0.0400(2) 0.00423(14) 0.00013(14) 0.00908(14) Br1 0.0476(3) 0.0460(3) 0.0618(4) 0.0073(2) 0.0020(3) -0.0015(2) C1 0.034(2) 0.050(3) 0.053(3) 0.003(2) 0.004(2) 0.018(2) C2 0.052(3) 0.055(3) 0.057(3) 0.005(3) 0.020(3) 0.021(3) C3 0.041(3) 0.064(4) 0.077(4) 0.023(3) 0.022(3) 0.013(3) C4 0.036(3) 0.042(3) 0.083(4) -0.008(3) -0.005(3) 0.004(2) C5 0.032(2) 0.061(3) 0.051(3) -0.007(2) -0.004(2) 0.017(2) C6 0.065(4) 0.058(4) 0.083(5) 0.015(3) 0.009(3) 0.031(3) C7 0.036(3) 0.055(3) 0.068(4) -0.002(3) -0.006(2) 0.016(2) O1 0.063(3) 0.093(4) 0.109(4) -0.019(3) 0.004(3) 0.047(3) C8 0.074(4) 0.043(3) 0.062(4) 0.007(3) -0.018(3) 0.013(3) O2 0.138(5) 0.070(3) 0.074(3) 0.009(3) -0.050(4) 0.028(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C8 1.881(6) . ? Ru1 C7 1.885(6) . ? Ru1 C4 2.184(5) . ? Ru1 C3 2.196(6) . ? Ru1 C2 2.231(6) . ? Ru1 C5 2.245(5) . ? Ru1 C1 2.303(5) . ? Ru1 Br1 2.5349(16) . ? C1 C5 1.415(7) . ? C1 C2 1.421(8) . ? C1 C6 1.487(9) . ? C2 C3 1.426(9) . ? C3 C4 1.402(9) . ? C4 C5 1.420(9) . ? C7 O1 1.127(7) . ? C8 O2 1.131(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 C8 Ru1 C7 90.4(3) . . ? C8 Ru1 C4 119.8(3) . . ? C7 Ru1 C4 95.4(2) . . ? C8 Ru1 C3 95.5(3) . . ? C7 Ru1 C3 126.2(3) . . ? C4 Ru1 C3 37.3(3) . . ? C8 Ru1 C2 105.7(3) . . ? C7 Ru1 C2 157.0(2) . . ? C4 Ru1 C2 62.5(2) . . ? C3 Ru1 C2 37.6(2) . . ? C8 Ru1 C5 156.3(3) . . ? C7 Ru1 C5 97.3(2) . . ? C4 Ru1 C5 37.4(2) . . ? C3 Ru1 C5 62.0(2) . . ? C2 Ru1 C5 61.6(2) . . ? C8 Ru1 C1 140.6(3) . . ? C7 Ru1 C1 128.9(2) . . ? C4 Ru1 C1 61.4(2) . . ? C3 Ru1 C1 61.4(2) . . ? C2 Ru1 C1 36.5(2) . . ? C5 Ru1 C1 36.24(19) . . ? C8 Ru1 Br1 88.8(2) . . ? C7 Ru1 Br1 92.64(19) . . ? C4 Ru1 Br1 150.15(19) . . ? C3 Ru1 Br1 140.72(18) . . ? C2 Ru1 Br1 103.83(16) . . ? C5 Ru1 Br1 113.05(17) . . ? C1 Ru1 Br1 91.43(14) . . ? C5 C1 C2 107.8(5) . . ? C5 C1 C6 124.9(5) . . ? C2 C1 C6 127.3(5) . . ? C5 C1 Ru1 69.6(3) . . ? C2 C1 Ru1 69.0(3) . . ? C6 C1 Ru1 126.4(4) . . ? C1 C2 C3 107.7(5) . . ? C1 C2 Ru1 74.5(3) . . ? C3 C2 Ru1 69.9(3) . . ? C4 C3 C2 108.1(6) . . ? C4 C3 Ru1 70.9(3) . . ? C2 C3 Ru1 72.6(3) . . ? C3 C4 C5 108.3(5) . . ? C3 C4 Ru1 71.8(3) . . ? C5 C4 Ru1 73.7(3) . . ? C1 C5 C4 108.0(5) . . ? C1 C5 Ru1 74.1(3) . . ? C4 C5 Ru1 69.0(3) . . ? O1 C7 Ru1 173.5(5) . . ? O2 C8 Ru1 178.2(6) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.035 _refine_diff_density_min -1.160 _refine_diff_density_rms 0.144 #===END data_jhn365a _database_code_CSD 195532 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 13 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H7 I O2 Ru' _chemical_formula_weight 363.11 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' O O 0.0106 0.0060 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.0680(17) _cell_length_b 7.538(2) _cell_length_c 10.2386(14) _cell_angle_alpha 92.931(18) _cell_angle_beta 96.106(13) _cell_angle_gamma 109.316(19) _cell_volume 509.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.76 _cell_measurement_theta_max 15.77 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max .19 _exptl_crystal_size_mid .42 _exptl_crystal_size_min .28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 4.525 _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 298(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3649 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 30.00 _reflns_number_total 2979 _reflns_number_gt 2332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1630P)^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 SHELXL _refine_ls_extinction_coef 0.010(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2979 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0984 _refine_ls_R_factor_gt 0.0845 _refine_ls_wR_factor_ref 0.2185 _refine_ls_wR_factor_gt 0.2023 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Ru1 Ru 0.52653(9) 0.22675(8) 0.23373(5) 0.0390(2) Uani 1 1 d . . . I1 I 0.23937(9) -0.11912(8) 0.21037(6) 0.0575(3) Uani 1 1 d . . . C1 C 0.7735(12) 0.1122(12) 0.3198(8) 0.0476(16) Uani 1 1 d . . . C2 C 0.7842(11) 0.2766(12) 0.3975(8) 0.0488(17) Uani 1 1 d . . . H2A H 0.7742 0.2851 0.4922 0.059 Uiso 1 1 calc R . . C3 C 0.8215(12) 0.4296(12) 0.3165(11) 0.057(2) Uani 1 1 d . . . H3A H 0.8504 0.5627 0.3463 0.068 Uiso 1 1 calc R . . C4 C 0.8374(14) 0.3568(14) 0.1888(11) 0.061(2) Uani 1 1 d . . . H4A H 0.8763 0.4318 0.1144 0.073 Uiso 1 1 calc R . . C5 C 0.8041(13) 0.1641(14) 0.1898(9) 0.0532(19) Uani 1 1 d . . . H5A H 0.8111 0.0805 0.1154 0.064 Uiso 1 1 calc R . . C6 C 0.7414(17) -0.0745(15) 0.3718(12) 0.070(3) Uani 1 1 d . . . H6A H 0.8699 -0.0860 0.4016 0.105 Uiso 1 1 calc R . . H6B H 0.6699 -0.1729 0.3033 0.105 Uiso 1 1 calc R . . H6C H 0.6637 -0.0851 0.4443 0.105 Uiso 1 1 calc R . . C7 C 0.3698(12) 0.3310(13) 0.3286(9) 0.0528(19) Uani 1 1 d . . . O1 O 0.2852(13) 0.4025(13) 0.3886(9) 0.085(3) Uani 1 1 d . . . C8 C 0.4016(15) 0.2728(13) 0.0736(9) 0.058(2) Uani 1 1 d . . . O2 O 0.3254(14) 0.3032(12) -0.0221(8) 0.088(3) Uani 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 Ru1 0.0389(4) 0.0357(3) 0.0379(3) -0.0010(2) -0.0014(2) 0.0092(2) I1 0.0523(4) 0.0494(4) 0.0537(4) 0.0008(2) 0.0027(3) -0.0035(3) C1 0.046(4) 0.052(4) 0.048(4) -0.002(3) 0.000(3) 0.023(3) C2 0.038(3) 0.056(4) 0.044(4) -0.012(3) -0.008(3) 0.011(3) C3 0.038(4) 0.040(4) 0.083(6) -0.009(4) -0.006(4) 0.008(3) C4 0.045(4) 0.055(5) 0.070(6) 0.016(4) 0.010(4) -0.001(4) C5 0.049(4) 0.063(5) 0.048(4) -0.002(4) 0.012(3) 0.019(4) C6 0.075(6) 0.060(6) 0.078(7) 0.019(5) 0.005(5) 0.025(5) C7 0.037(4) 0.059(5) 0.062(5) -0.013(4) -0.005(3) 0.022(4) O1 0.074(5) 0.088(6) 0.100(6) -0.026(5) 0.006(5) 0.044(5) C8 0.060(5) 0.044(4) 0.056(5) 0.007(3) -0.013(4) 0.005(4) O2 0.093(6) 0.077(5) 0.070(5) 0.013(4) -0.035(5) 0.012(5) _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 C7 1.874(8) . ? Ru1 C8 1.882(9) . ? Ru1 C3 2.188(8) . ? Ru1 C4 2.199(9) . ? Ru1 C5 2.248(8) . ? Ru1 C2 2.259(7) . ? Ru1 C1 2.306(8) . ? Ru1 I1 2.7030(11) . ? C1 C2 1.413(11) . ? C1 C5 1.425(12) . ? C1 C6 1.485(13) . ? C2 C3 1.425(14) . ? C3 C4 1.422(16) . ? C4 C5 1.394(14) . ? C7 O1 1.133(10) . ? C8 O2 1.138(11) . ? 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 C7 Ru1 C8 90.6(4) . . ? C7 Ru1 C3 96.9(4) . . ? C8 Ru1 C3 118.1(4) . . ? C7 Ru1 C4 129.7(4) . . ? C8 Ru1 C4 95.3(4) . . ? C3 Ru1 C4 37.8(4) . . ? C7 Ru1 C5 157.0(3) . . ? C8 Ru1 C5 107.2(4) . . ? C3 Ru1 C5 62.1(3) . . ? C4 Ru1 C5 36.5(4) . . ? C7 Ru1 C2 96.9(3) . . ? C8 Ru1 C2 154.9(4) . . ? C3 Ru1 C2 37.3(4) . . ? C4 Ru1 C2 61.7(4) . . ? C5 Ru1 C2 60.9(3) . . ? C7 Ru1 C1 126.9(3) . . ? C8 Ru1 C1 142.4(4) . . ? C3 Ru1 C1 61.7(3) . . ? C4 Ru1 C1 61.0(3) . . ? C5 Ru1 C1 36.4(3) . . ? C2 Ru1 C1 36.0(3) . . ? C7 Ru1 I1 91.6(3) . . ? C8 Ru1 I1 88.2(3) . . ? C3 Ru1 I1 152.2(3) . . ? C4 Ru1 I1 138.4(3) . . ? C5 Ru1 I1 103.1(3) . . ? C2 Ru1 I1 115.4(2) . . ? C1 Ru1 I1 92.2(2) . . ? C2 C1 C5 107.2(8) . . ? C2 C1 C6 123.9(8) . . ? C5 C1 C6 128.9(8) . . ? C2 C1 Ru1 70.2(4) . . ? C5 C1 Ru1 69.5(5) . . ? C6 C1 Ru1 126.7(7) . . ? C1 C2 C3 108.6(8) . . ? C1 C2 Ru1 73.8(4) . . ? C3 C2 Ru1 68.6(5) . . ? C4 C3 C2 106.8(8) . . ? C4 C3 Ru1 71.5(5) . . ? C2 C3 Ru1 74.1(5) . . ? C5 C4 C3 108.8(8) . . ? C5 C4 Ru1 73.7(5) . . ? C3 C4 Ru1 70.7(5) . . ? C4 C5 C1 108.6(8) . . ? C4 C5 Ru1 69.8(5) . . ? C1 C5 Ru1 74.0(5) . . ? O1 C7 Ru1 176.0(8) . . ? O2 C8 Ru1 178.8(10) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 4.155 _refine_diff_density_min -4.038 _refine_diff_density_rms 0.431 #===END data_jhn369a _database_code_CSD 195533 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 14 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H20 Br O P Ru' _chemical_formula_weight 500.32 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' O O 0.0106 0.0060 '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' Br Br -0.2901 2.4595 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.665(2) _cell_length_b 14.513(4) _cell_length_c 14.740(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.747(18) _cell_angle_gamma 90.00 _cell_volume 1999.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 5.22 _cell_measurement_theta_max 12.37 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max .20 _exptl_crystal_size_mid .46 _exptl_crystal_size_min .44 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 2.868 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8216 _exptl_absorpt_correction_T_max 0.9762 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4563 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3528 _reflns_number_gt 2098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^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_number_reflns 3528 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1284 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1839 _refine_ls_wR_factor_gt 0.1509 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Ru1 Ru 0.17361(9) 0.82423(6) 0.21172(5) 0.0409(3) Uani 1 1 d . . . Br1 Br 0.28658(13) 0.98057(8) 0.19979(8) 0.0651(4) Uani 1 1 d . . . P1 P 0.1184(3) 0.87190(19) 0.34651(17) 0.0425(6) Uani 1 1 d . . . C1 C 0.0754(16) 0.8234(9) 0.0547(7) 0.071(4) Uani 1 1 d . . . C2 C 0.1416(13) 0.7409(9) 0.0792(8) 0.062(3) Uani 1 1 d . . . H2A H 0.2187 0.7161 0.0543 0.075 Uiso 1 1 calc R . . C3 C 0.0815(13) 0.6957(7) 0.1456(7) 0.058(3) Uani 1 1 d . . . H3A H 0.1023 0.6332 0.1703 0.069 Uiso 1 1 calc R . . C4 C -0.0321(13) 0.7553(8) 0.1571(8) 0.063(3) Uani 1 1 d . . . H4A H -0.1015 0.7407 0.1932 0.075 Uiso 1 1 calc R . . C5 C -0.0317(12) 0.8356(8) 0.1036(8) 0.063(3) Uani 1 1 d . . . H5A H -0.0999 0.8868 0.0958 0.076 Uiso 1 1 calc R . . C6 C 0.1077(18) 0.8918(10) -0.0150(9) 0.112(6) Uani 1 1 d . . . H6A H 0.0529 0.8763 -0.0771 0.167 Uiso 1 1 calc R . . H6B H 0.2078 0.8897 -0.0127 0.167 Uiso 1 1 calc R . . H6C H 0.0827 0.9528 0.0005 0.167 Uiso 1 1 calc R . . C7 C 0.2451(15) 0.9487(9) 0.4220(8) 0.077(4) Uani 1 1 d . . . H7A H 0.2587 0.9964 0.3829 0.092 Uiso 1 1 calc R . . C8 C 0.305(3) 0.964(3) 0.4823(15) 0.33(3) Uani 1 1 d . . . H8A H 0.3080 0.9253 0.5331 0.391 Uiso 1 1 calc R . . H8B H 0.3591 1.0176 0.4903 0.391 Uiso 1 1 calc R . . C9 C 0.0938(10) 0.7833(8) 0.4295(7) 0.045(2) Uani 1 1 d . . . C10 C 0.1013(11) 0.6918(8) 0.4109(7) 0.054(3) Uani 1 1 d . . . H10A H 0.1235 0.6738 0.3558 0.065 Uiso 1 1 calc R . . C11 C 0.0768(13) 0.6248(9) 0.4719(8) 0.072(3) Uani 1 1 d . . . H11A H 0.0821 0.5625 0.4580 0.086 Uiso 1 1 calc R . . C12 C 0.0445(13) 0.6524(9) 0.5537(8) 0.068(4) Uani 1 1 d . . . H12A H 0.0263 0.6084 0.5951 0.082 Uiso 1 1 calc R . . C13 C 0.0389(14) 0.7430(10) 0.5744(8) 0.075(4) Uani 1 1 d . . . H13A H 0.0183 0.7605 0.6303 0.091 Uiso 1 1 calc R . . C14 C 0.0631(13) 0.8088(8) 0.5141(8) 0.064(3) Uani 1 1 d . . . H14A H 0.0593 0.8708 0.5292 0.077 Uiso 1 1 calc R . . C15 C -0.0508(11) 0.9344(7) 0.3182(7) 0.050(3) Uani 1 1 d . . . C16 C -0.1793(13) 0.8963(8) 0.3279(8) 0.064(3) Uani 1 1 d . . . H16A H -0.1789 0.8384 0.3549 0.076 Uiso 1 1 calc R . . C17 C -0.3065(14) 0.9436(11) 0.2981(9) 0.074(4) Uani 1 1 d . . . H17A H -0.3913 0.9177 0.3048 0.089 Uiso 1 1 calc R . . C18 C -0.3068(15) 1.0285(10) 0.2586(9) 0.073(4) Uani 1 1 d . . . H18A H -0.3931 1.0599 0.2386 0.088 Uiso 1 1 calc R . . C19 C -0.1859(15) 1.0686(9) 0.2475(9) 0.074(4) Uani 1 1 d . . . H19A H -0.1883 1.1268 0.2207 0.089 Uiso 1 1 calc R . . C20 C -0.0569(13) 1.0202(9) 0.2774(8) 0.065(3) Uani 1 1 d . . . H20A H 0.0268 1.0467 0.2694 0.078 Uiso 1 1 calc R . . C21 C 0.3494(15) 0.7735(9) 0.2815(8) 0.056(3) Uani 1 1 d . . . O1 O 0.4445(10) 0.7473(7) 0.3175(6) 0.080(3) Uani 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 Ru1 0.0509(5) 0.0398(5) 0.0367(4) 0.0013(4) 0.0198(3) 0.0002(4) Br1 0.0778(9) 0.0610(8) 0.0656(8) -0.0018(6) 0.0349(7) -0.0182(7) P1 0.0495(16) 0.0441(15) 0.0388(14) -0.0023(12) 0.0201(12) -0.0052(13) C1 0.120(11) 0.061(8) 0.036(6) 0.003(6) 0.025(7) -0.017(9) C2 0.063(8) 0.067(9) 0.062(7) -0.024(6) 0.027(6) -0.004(7) C3 0.087(9) 0.030(6) 0.057(7) -0.007(5) 0.019(6) -0.010(6) C4 0.071(8) 0.061(8) 0.059(7) -0.011(6) 0.023(6) -0.022(7) C5 0.047(7) 0.060(8) 0.073(8) 0.002(6) -0.002(6) 0.008(6) C6 0.183(17) 0.098(12) 0.054(8) 0.014(8) 0.031(10) -0.034(12) C7 0.109(11) 0.083(9) 0.040(6) -0.015(6) 0.021(7) -0.058(8) C8 0.38(4) 0.53(6) 0.093(15) -0.12(2) 0.10(2) -0.38(4) C9 0.038(6) 0.058(7) 0.042(6) -0.002(5) 0.015(5) -0.007(5) C10 0.060(7) 0.061(8) 0.047(6) 0.007(5) 0.025(5) 0.003(6) C11 0.101(10) 0.059(8) 0.064(8) -0.001(6) 0.036(7) -0.012(7) C12 0.083(9) 0.072(9) 0.053(7) 0.014(6) 0.022(6) -0.022(7) C13 0.094(10) 0.100(11) 0.050(7) 0.002(7) 0.050(7) -0.029(8) C14 0.083(8) 0.061(8) 0.059(7) -0.009(6) 0.038(6) -0.007(7) C15 0.063(7) 0.046(6) 0.044(6) -0.004(5) 0.022(5) 0.006(6) C16 0.072(8) 0.058(8) 0.069(7) -0.001(6) 0.034(7) -0.008(7) C17 0.066(9) 0.086(10) 0.072(9) 0.002(8) 0.022(7) -0.001(8) C18 0.075(9) 0.081(10) 0.066(8) -0.019(7) 0.020(7) 0.015(8) C19 0.090(10) 0.070(9) 0.064(8) -0.011(7) 0.023(7) 0.009(9) C20 0.067(8) 0.071(9) 0.060(7) -0.005(6) 0.022(6) 0.001(7) C21 0.076(9) 0.053(7) 0.050(7) -0.005(6) 0.036(7) -0.007(7) O1 0.079(7) 0.091(7) 0.074(6) 0.033(5) 0.026(5) 0.027(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 Ru1 C21 1.897(15) . ? Ru1 C3 2.186(10) . ? Ru1 C4 2.188(11) . ? Ru1 C5 2.212(10) . ? Ru1 C2 2.251(11) . ? Ru1 C1 2.267(11) . ? Ru1 P1 2.292(2) . ? Ru1 Br1 2.5433(15) . ? P1 C7 1.813(12) . ? P1 C15 1.823(11) . ? P1 C9 1.831(11) . ? C1 C2 1.363(16) . ? C1 C5 1.414(16) . ? C1 C6 1.517(16) . ? C2 C3 1.419(15) . ? C3 C4 1.441(16) . ? C4 C5 1.409(16) . ? C7 C8 0.95(2) . ? C9 C10 1.361(14) . ? C9 C14 1.404(14) . ? C10 C11 1.385(15) . ? C11 C12 1.381(15) . ? C12 C13 1.353(17) . ? C13 C14 1.366(15) . ? C15 C20 1.379(15) . ? C15 C16 1.399(14) . ? C16 C17 1.378(16) . ? C17 C18 1.362(18) . ? C18 C19 1.353(17) . ? C19 C20 1.400(16) . ? C21 O1 1.011(13) . ? 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 C21 Ru1 C3 96.7(5) . . ? C21 Ru1 C4 128.8(5) . . ? C3 Ru1 C4 38.5(4) . . ? C21 Ru1 C5 159.2(5) . . ? C3 Ru1 C5 63.5(4) . . ? C4 Ru1 C5 37.3(4) . . ? C21 Ru1 C2 99.7(5) . . ? C3 Ru1 C2 37.3(4) . . ? C4 Ru1 C2 61.5(4) . . ? C5 Ru1 C2 61.0(4) . . ? C21 Ru1 C1 129.5(5) . . ? C3 Ru1 C1 61.5(4) . . ? C4 Ru1 C1 61.1(4) . . ? C5 Ru1 C1 36.8(4) . . ? C2 Ru1 C1 35.1(4) . . ? C21 Ru1 P1 91.2(3) . . ? C3 Ru1 P1 119.1(3) . . ? C4 Ru1 P1 93.8(3) . . ? C5 Ru1 P1 103.8(3) . . ? C2 Ru1 P1 154.6(3) . . ? C1 Ru1 P1 139.2(4) . . ? C21 Ru1 Br1 92.5(4) . . ? C3 Ru1 Br1 149.7(3) . . ? C4 Ru1 Br1 138.5(3) . . ? C5 Ru1 Br1 101.9(3) . . ? C2 Ru1 Br1 112.7(3) . . ? C1 Ru1 Br1 90.5(3) . . ? P1 Ru1 Br1 89.40(8) . . ? C7 P1 C15 105.1(6) . . ? C7 P1 C9 101.8(5) . . ? C15 P1 C9 104.0(5) . . ? C7 P1 Ru1 116.6(4) . . ? C15 P1 Ru1 110.2(3) . . ? C9 P1 Ru1 117.7(4) . . ? C2 C1 C5 109.2(10) . . ? C2 C1 C6 126.3(13) . . ? C5 C1 C6 124.5(14) . . ? C2 C1 Ru1 71.8(6) . . ? C5 C1 Ru1 69.5(6) . . ? C6 C1 Ru1 125.7(9) . . ? C1 C2 C3 110.0(11) . . ? C1 C2 Ru1 73.1(6) . . ? C3 C2 Ru1 68.9(6) . . ? C2 C3 C4 105.2(10) . . ? C2 C3 Ru1 73.8(6) . . ? C4 C3 Ru1 70.8(6) . . ? C5 C4 C3 108.6(10) . . ? C5 C4 Ru1 72.3(6) . . ? C3 C4 Ru1 70.7(6) . . ? C4 C5 C1 106.8(11) . . ? C4 C5 Ru1 70.4(7) . . ? C1 C5 Ru1 73.7(7) . . ? C8 C7 P1 150(2) . . ? C10 C9 C14 118.0(10) . . ? C10 C9 P1 121.9(8) . . ? C14 C9 P1 120.1(9) . . ? C9 C10 C11 121.9(10) . . ? C12 C11 C10 118.5(12) . . ? C13 C12 C11 120.7(11) . . ? C12 C13 C14 120.7(11) . . ? C13 C14 C9 120.3(11) . . ? C20 C15 C16 117.4(11) . . ? C20 C15 P1 119.1(9) . . ? C16 C15 P1 123.2(9) . . ? C17 C16 C15 120.9(12) . . ? C18 C17 C16 119.5(13) . . ? C19 C18 C17 122.2(13) . . ? C18 C19 C20 118.3(13) . . ? C15 C20 C19 121.7(12) . . ? O1 C21 Ru1 178.4(12) . . ? _diffrn_measured_fraction_theta_max 0.864 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.864 _refine_diff_density_max 1.201 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.132 #===END