data_publication_text _publ_requested_journal Journal of The Americal Chemical Society _publ_contact_author_name 'Robert H. Grubbs' _publ_contact_author_address ;California Institute of Technology 1200 E. California Blvd. Pasadena, CA 91125 (USA) ; _publ_contact_author_email rhg@caltech.edu _publ_contact_author_phone 1(626)3956003 _publ_contact_author_fax 1(626)5649297 data_ckc02 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H38 Cl2 N2 O Ru' _chemical_formula_sum 'C31 H38 Cl2 N2 O Ru' _chemical_formula_weight 626.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1757(3) _cell_length_b 10.6130(4) _cell_length_c 16.2638(6) _cell_angle_alpha 85.3300(10) _cell_angle_beta 77.2650(10) _cell_angle_gamma 72.2060(10) _cell_volume 1470.76(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17086 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 41.27 _exptl_crystal_description Blade _exptl_crystal_colour 'Dichroic - light green / dark blue' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7975 _exptl_absorpt_correction_T_max 0.9229 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 SMART 1000' _diffrn_measurement_method '\w scans at 8 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45559 _diffrn_reflns_av_R_equivalents 0.0938 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 41.86 _reflns_number_total 16192 _reflns_number_gt 11711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.630' _computing_cell_refinement 'Bruker SAINT v6.45A' _computing_data_reduction 'Bruker SAINT v6.45A' _computing_structure_solution 'Bruker XS v6.12' _computing_structure_refinement 'Bruker XL v6.12' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF v6.12' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16192 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.0937 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_restrained_S_all 1.187 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.721709(15) 0.813032(14) 0.708710(9) 0.01269(3) Uani 1 1 d . . . Cl1 Cl 0.78533(5) 0.94386(5) 0.79755(3) 0.02051(8) Uani 1 1 d . . . Cl2 Cl 0.57543(5) 0.71106(5) 0.64899(3) 0.01774(8) Uani 1 1 d . . . O1 O 0.61694(15) 0.99428(13) 0.63370(8) 0.0197(2) Uani 1 1 d . . . N1 N 0.71098(16) 0.62639(15) 0.84842(9) 0.0167(3) Uani 1 1 d . . . N2 N 0.90858(16) 0.53153(15) 0.74937(10) 0.0170(3) Uani 1 1 d . . . C1 C 0.79616(18) 0.64806(18) 0.77133(10) 0.0146(3) Uani 1 1 d . . . C2 C 0.7361(2) 0.48019(19) 0.86707(12) 0.0218(3) Uani 1 1 d . . . C3 C 0.9058(2) 0.4234(2) 0.81434(13) 0.0233(4) Uani 1 1 d . . . C4 C 0.7200(3) 0.4483(2) 0.96108(13) 0.0290(4) Uani 1 1 d . . . H4A H 0.7950 0.4782 0.9829 0.044 Uiso 1 1 calc R . . H4B H 0.7412 0.3525 0.9702 0.044 Uiso 1 1 calc R . . H4C H 0.6135 0.4935 0.9907 0.044 Uiso 1 1 calc R . . C5 C 0.6155(2) 0.4369(2) 0.83333(14) 0.0274(4) Uani 1 1 d . . . H5A H 0.5100 0.4831 0.8637 0.041 Uiso 1 1 calc R . . H5B H 0.6347 0.3412 0.8417 0.041 Uiso 1 1 calc R . . H5C H 0.6248 0.4589 0.7731 0.041 Uiso 1 1 calc R . . C6 C 1.0317(2) 0.4117(3) 0.86422(15) 0.0318(5) Uani 1 1 d . . . H6A H 1.1346 0.3876 0.8262 0.048 Uiso 1 1 calc R . . H6B H 1.0279 0.3433 0.9082 0.048 Uiso 1 1 calc R . . H6C H 1.0135 0.4967 0.8903 0.048 Uiso 1 1 calc R . . C7 C 0.9337(3) 0.2896(2) 0.77527(15) 0.0307(5) Uani 1 1 d . . . H7A H 0.8604 0.2988 0.7379 0.046 Uiso 1 1 calc R . . H7B H 0.9174 0.2248 0.8201 0.046 Uiso 1 1 calc R . . H7C H 1.0413 0.2595 0.7427 0.046 Uiso 1 1 calc R . . C8 C 0.56902(19) 0.72217(18) 0.88899(11) 0.0171(3) Uani 1 1 d . . . C9 C 0.5673(2) 0.7835(2) 0.96319(12) 0.0225(4) Uani 1 1 d . . . C10 C 0.4247(3) 0.8692(2) 1.00392(13) 0.0289(4) Uani 1 1 d . . . H10 H 0.4204 0.9099 1.0547 0.035 Uiso 1 1 calc R . . C11 C 0.2898(2) 0.8961(2) 0.97209(14) 0.0291(4) Uani 1 1 d . . . H11 H 0.1949 0.9549 1.0008 0.035 Uiso 1 1 calc R . . C12 C 0.2934(2) 0.8370(2) 0.89813(14) 0.0270(4) Uani 1 1 d . . . H12 H 0.2018 0.8563 0.8755 0.032 Uiso 1 1 calc R . . C13 C 0.4331(2) 0.7490(2) 0.85753(12) 0.0208(3) Uani 1 1 d . . . H13 H 0.4355 0.7068 0.8077 0.025 Uiso 1 1 calc R . . C14 C 0.7122(3) 0.7606(2) 0.99822(15) 0.0323(5) Uani 1 1 d . . . H14A H 0.6955 0.8305 1.0382 0.048 Uiso 1 1 calc R . . H14B H 0.8007 0.7621 0.9521 0.048 Uiso 1 1 calc R . . H14C H 0.7348 0.6744 1.0272 0.048 Uiso 1 1 calc R . . C15 C 1.04182(18) 0.51680(17) 0.68069(11) 0.0150(3) Uani 1 1 d . . . C16 C 1.16291(19) 0.56981(18) 0.68413(11) 0.0167(3) Uani 1 1 d . . . C17 C 1.28900(19) 0.5493(2) 0.61548(12) 0.0212(4) Uani 1 1 d . . . H17 H 1.3718 0.5851 0.6160 0.025 Uiso 1 1 calc R . . C18 C 1.2956(2) 0.4773(2) 0.54643(13) 0.0258(4) Uani 1 1 d . . . H18 H 1.3829 0.4638 0.5005 0.031 Uiso 1 1 calc R . . C19 C 1.1750(2) 0.4251(2) 0.54426(13) 0.0248(4) Uani 1 1 d . . . H19 H 1.1796 0.3757 0.4971 0.030 Uiso 1 1 calc R . . C20 C 1.0474(2) 0.44543(19) 0.61157(12) 0.0194(3) Uani 1 1 d . . . H20 H 0.9642 0.4105 0.6103 0.023 Uiso 1 1 calc R . . C21 C 1.1574(2) 0.6529(2) 0.75547(14) 0.0299(5) Uani 1 1 d . . . H21A H 1.1997 0.5956 0.8003 0.045 Uiso 1 1 calc R . . H21B H 1.0488 0.7041 0.7776 0.045 Uiso 1 1 calc R . . H21C H 1.2201 0.7135 0.7352 0.045 Uiso 1 1 calc R . . C22 C 0.87944(19) 0.79945(17) 0.61508(11) 0.0162(3) Uani 1 1 d . . . H22 H 0.9787 0.7358 0.6133 0.019 Uiso 1 1 calc R . . C23 C 0.8491(2) 0.88798(18) 0.54400(11) 0.0165(3) Uani 1 1 d . . . C24 C 0.9541(2) 0.8743(2) 0.46540(12) 0.0218(3) Uani 1 1 d . . . H24 H 1.0511 0.8061 0.4580 0.026 Uiso 1 1 calc R . . C25 C 0.9170(3) 0.9595(2) 0.39875(12) 0.0268(4) Uani 1 1 d . . . H25 H 0.9878 0.9500 0.3458 0.032 Uiso 1 1 calc R . . C26 C 0.7752(3) 1.0590(2) 0.41034(13) 0.0281(4) Uani 1 1 d . . . H26 H 0.7496 1.1166 0.3644 0.034 Uiso 1 1 calc R . . C27 C 0.6693(2) 1.0766(2) 0.48748(13) 0.0248(4) Uani 1 1 d . . . H27 H 0.5731 1.1455 0.4945 0.030 Uiso 1 1 calc R . . C28 C 0.7079(2) 0.99086(19) 0.55377(12) 0.0188(3) Uani 1 1 d . . . C29 C 0.4874(2) 1.1139(2) 0.66161(14) 0.0281(4) Uani 1 1 d . . . H29 H 0.4211 1.1412 0.6182 0.034 Uiso 1 1 calc R . . C30 C 0.5537(3) 1.2254(2) 0.67304(18) 0.0415(6) Uani 1 1 d . . . H30A H 0.6278 1.1952 0.7108 0.062 Uiso 1 1 calc R . . H30B H 0.4683 1.3021 0.6975 0.062 Uiso 1 1 calc R . . H30C H 0.6078 1.2505 0.6182 0.062 Uiso 1 1 calc R . . C31 C 0.3925(3) 1.0739(3) 0.74244(15) 0.0353(5) Uani 1 1 d . . . H31A H 0.3598 0.9980 0.7318 0.053 Uiso 1 1 calc R . . H31B H 0.2998 1.1482 0.7623 0.053 Uiso 1 1 calc R . . H31C H 0.4566 1.0495 0.7855 0.053 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 0.01108(5) 0.01367(6) 0.01340(6) -0.00137(4) -0.00272(4) -0.00334(4) Cl1 0.02344(19) 0.0201(2) 0.02024(19) -0.00500(16) -0.00574(15) -0.00757(16) Cl2 0.01630(16) 0.0243(2) 0.01576(17) -0.00206(15) -0.00396(13) -0.00963(15) O1 0.0190(6) 0.0165(6) 0.0208(6) 0.0011(5) -0.0051(5) -0.0011(5) N1 0.0124(6) 0.0181(7) 0.0161(6) 0.0015(5) -0.0001(5) -0.0018(5) N2 0.0129(6) 0.0165(7) 0.0182(7) 0.0020(5) 0.0002(5) -0.0023(5) C1 0.0120(6) 0.0189(8) 0.0130(6) -0.0015(6) -0.0014(5) -0.0050(6) C2 0.0191(7) 0.0193(8) 0.0222(8) 0.0029(7) 0.0016(6) -0.0037(7) C3 0.0167(7) 0.0216(9) 0.0269(9) 0.0023(7) 0.0005(6) -0.0029(7) C4 0.0297(10) 0.0282(10) 0.0229(9) 0.0062(8) 0.0016(7) -0.0061(8) C5 0.0244(9) 0.0258(10) 0.0308(10) -0.0054(8) 0.0042(7) -0.0112(8) C6 0.0213(9) 0.0399(13) 0.0322(11) 0.0073(10) -0.0080(8) -0.0065(9) C7 0.0284(10) 0.0200(9) 0.0389(12) -0.0015(8) 0.0018(9) -0.0061(8) C8 0.0149(7) 0.0190(8) 0.0142(7) 0.0001(6) 0.0006(5) -0.0029(6) C9 0.0255(8) 0.0229(9) 0.0190(8) -0.0011(7) -0.0022(7) -0.0084(7) C10 0.0368(11) 0.0253(10) 0.0207(9) -0.0058(8) 0.0054(8) -0.0100(9) C11 0.0243(9) 0.0227(10) 0.0303(10) -0.0040(8) 0.0082(8) -0.0014(8) C12 0.0162(7) 0.0288(10) 0.0286(10) 0.0006(8) 0.0018(7) -0.0008(7) C13 0.0159(7) 0.0263(9) 0.0171(8) -0.0013(7) 0.0000(6) -0.0039(7) C14 0.0378(11) 0.0357(12) 0.0295(11) -0.0009(9) -0.0166(9) -0.0129(10) C15 0.0103(6) 0.0162(7) 0.0162(7) -0.0006(6) -0.0008(5) -0.0019(6) C16 0.0136(6) 0.0181(8) 0.0183(7) -0.0034(6) -0.0031(5) -0.0036(6) C17 0.0124(6) 0.0270(9) 0.0252(9) -0.0063(7) -0.0014(6) -0.0074(7) C18 0.0182(8) 0.0344(11) 0.0241(9) -0.0095(8) 0.0060(7) -0.0116(8) C19 0.0221(8) 0.0322(11) 0.0221(9) -0.0096(8) 0.0014(7) -0.0125(8) C20 0.0163(7) 0.0226(9) 0.0208(8) -0.0033(7) -0.0024(6) -0.0081(7) C21 0.0253(9) 0.0364(12) 0.0313(11) -0.0105(9) -0.0027(8) -0.0137(9) C22 0.0168(7) 0.0160(7) 0.0170(7) 0.0009(6) -0.0049(6) -0.0061(6) C23 0.0191(7) 0.0174(8) 0.0163(7) 0.0028(6) -0.0051(6) -0.0097(6) C24 0.0260(8) 0.0243(9) 0.0185(8) 0.0012(7) -0.0027(6) -0.0140(7) C25 0.0382(11) 0.0324(11) 0.0167(8) 0.0047(8) -0.0058(7) -0.0219(9) C26 0.0418(11) 0.0286(10) 0.0233(9) 0.0100(8) -0.0163(8) -0.0200(9) C27 0.0295(9) 0.0219(9) 0.0273(10) 0.0082(7) -0.0142(8) -0.0103(8) C28 0.0215(8) 0.0182(8) 0.0196(8) 0.0026(6) -0.0083(6) -0.0082(7) C29 0.0248(9) 0.0215(9) 0.0325(11) -0.0017(8) -0.0099(8) 0.0043(8) C30 0.0593(16) 0.0185(10) 0.0458(14) -0.0050(10) -0.0175(12) -0.0044(11) C31 0.0227(9) 0.0391(13) 0.0324(11) -0.0052(10) -0.0050(8) 0.0085(9) _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 C22 1.8360(17) . yes Ru1 C1 1.9633(18) . yes Ru1 O1 2.2621(14) . yes Ru1 Cl1 2.3559(4) . yes Ru1 Cl2 2.3559(4) . yes O1 C28 1.378(2) . ? O1 C29 1.472(2) . ? N1 C1 1.366(2) . ? N1 C8 1.444(2) . ? N1 C2 1.513(2) . ? N2 C1 1.360(2) . ? N2 C15 1.441(2) . ? N2 C3 1.497(3) . ? C2 C4 1.524(3) . ? C2 C5 1.535(3) . ? C2 C3 1.564(2) . ? C3 C6 1.522(3) . ? C3 C7 1.529(3) . ? C8 C13 1.393(3) . ? C8 C9 1.412(3) . ? C9 C10 1.402(3) . ? C9 C14 1.506(3) . ? C10 C11 1.387(3) . ? C11 C12 1.391(3) . ? C12 C13 1.395(3) . ? C15 C20 1.389(2) . ? C15 C16 1.403(2) . ? C16 C17 1.396(2) . ? C16 C21 1.497(3) . ? C17 C18 1.389(3) . ? C18 C19 1.389(3) . ? C19 C20 1.391(2) . ? C22 C23 1.450(3) . ? C23 C28 1.403(3) . ? C23 C24 1.409(2) . ? C24 C25 1.387(3) . ? C25 C26 1.388(3) . ? C26 C27 1.394(3) . ? C27 C28 1.388(3) . ? C29 C31 1.516(3) . ? C29 C30 1.527(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C22 Ru1 C1 103.04(7) . . yes C22 Ru1 O1 79.01(7) . . yes C1 Ru1 O1 174.03(6) . . yes C22 Ru1 Cl1 101.89(5) . . yes C1 Ru1 Cl1 94.04(5) . . yes O1 Ru1 Cl1 90.99(4) . . yes C22 Ru1 Cl2 95.85(5) . . yes C1 Ru1 Cl2 88.98(5) . . yes O1 Ru1 Cl2 85.21(4) . . yes Cl1 Ru1 Cl2 160.813(16) . . yes C28 O1 C29 119.65(15) . . ? C28 O1 Ru1 110.00(11) . . ? C29 O1 Ru1 129.75(12) . . ? C1 N1 C8 123.11(15) . . ? C1 N1 C2 111.54(14) . . ? C8 N1 C2 120.22(14) . . ? C1 N2 C15 124.44(15) . . ? C1 N2 C3 114.11(14) . . ? C15 N2 C3 119.97(14) . . ? N2 C1 N1 106.23(15) . . ? N2 C1 Ru1 133.02(12) . . ? N1 C1 Ru1 119.76(12) . . ? N1 C2 C4 112.12(16) . . ? N1 C2 C5 108.57(16) . . ? C4 C2 C5 109.54(16) . . ? N1 C2 C3 99.90(14) . . ? C4 C2 C3 114.01(17) . . ? C5 C2 C3 112.30(16) . . ? N2 C3 C6 109.06(16) . . ? N2 C3 C7 112.41(17) . . ? C6 C3 C7 108.98(18) . . ? N2 C3 C2 99.85(15) . . ? C6 C3 C2 113.13(17) . . ? C7 C3 C2 113.16(16) . . ? C13 C8 C9 120.25(16) . . ? C13 C8 N1 120.29(15) . . ? C9 C8 N1 119.39(16) . . ? C10 C9 C8 117.76(19) . . ? C10 C9 C14 120.06(19) . . ? C8 C9 C14 122.17(18) . . ? C11 C10 C9 121.73(19) . . ? C10 C11 C12 120.07(18) . . ? C11 C12 C13 119.2(2) . . ? C8 C13 C12 120.95(18) . . ? C20 C15 C16 121.21(15) . . ? C20 C15 N2 117.33(15) . . ? C16 C15 N2 121.44(15) . . ? C17 C16 C15 117.81(15) . . ? C17 C16 C21 119.32(16) . . ? C15 C16 C21 122.77(15) . . ? C18 C17 C16 121.20(16) . . ? C19 C18 C17 120.20(16) . . ? C18 C19 C20 119.61(17) . . ? C15 C20 C19 119.96(16) . . ? C23 C22 Ru1 118.53(13) . . ? C28 C23 C24 118.66(17) . . ? C28 C23 C22 118.41(16) . . ? C24 C23 C22 122.92(17) . . ? C25 C24 C23 120.48(19) . . ? C24 C25 C26 119.27(19) . . ? C25 C26 C27 121.83(19) . . ? C28 C27 C26 118.38(19) . . ? O1 C28 C27 125.80(17) . . ? O1 C28 C23 112.83(16) . . ? C27 C28 C23 121.36(17) . . ? O1 C29 C31 105.52(17) . . ? O1 C29 C30 109.35(18) . . ? C31 C29 C30 113.5(2) . . ? _diffrn_measured_fraction_theta_max 0.794 _diffrn_reflns_theta_full 41.86 _diffrn_measured_fraction_theta_full 0.794 _refine_diff_density_max 2.317 _refine_diff_density_min -1.637 _refine_diff_density_rms 0.128 #===END data_ckc03 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H44 N2 O Cl2 Ru, 0.5(C5 H12)' _chemical_formula_sum 'C36.50 H49.50 Cl2 N2 O Ru' _chemical_formula_weight 704.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5182(8) _cell_length_b 12.3831(8) _cell_length_c 12.4144(8) _cell_angle_alpha 99.737(3) _cell_angle_beta 92.627(4) _cell_angle_gamma 92.065(4) _cell_volume 1741.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9852 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 30.72 _exptl_crystal_description Plate _exptl_crystal_colour Blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 737 _exptl_absorpt_coefficient_mu 0.634 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8040 _exptl_absorpt_correction_T_max 0.8999 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 KAPPA APEX II' _diffrn_measurement_method '\w and \f scans; 6 settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29761 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 31.98 _reflns_number_total 10056 _reflns_number_gt 7915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX22 v2.1-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.34A' _computing_data_reduction 'Bruker SAINT-Plus v7.34A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF v6.12' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10056 _refine_ls_number_parameters 428 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 2.665 _refine_ls_restrained_S_all 2.665 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.80580(4) 0.76118(3) 0.70308(3) 0.01588(10) Uani 0.9365(16) 1 d P A 1 Cl1 Cl 0.87830(8) 0.79412(7) 0.88440(6) 0.0261(2) Uani 0.9365(16) 1 d P A 1 Cl2 Cl 0.78944(8) 0.75957(7) 0.51386(6) 0.0265(2) Uani 0.9365(16) 1 d P A 1 Cl2B Cl 0.756(2) 0.7187(19) 0.9288(18) 0.096(8) Uani 0.0635(16) 1 d PU A 2 Cl1B Cl 0.7204(17) 0.6709(16) 0.5509(17) 0.100(9) Uani 0.0635(16) 1 d P A 2 Ru2 Ru 0.7541(7) 0.7243(7) 0.7395(9) 0.074(4) Uani 0.0635(16) 1 d P A 2 O1 O 0.96193(18) 0.65906(17) 0.66656(17) 0.0270(5) Uani 1 1 d . A 1 N1 N 0.6922(2) 0.96813(19) 0.74930(19) 0.0200(6) Uani 1 1 d . A 1 N2 N 0.5572(2) 0.83780(19) 0.74327(19) 0.0207(6) Uani 1 1 d . A 1 C1 C 0.6739(3) 0.8563(2) 0.7342(2) 0.0199(7) Uani 1 1 d . A 1 C2 C 0.5890(4) 1.0264(3) 0.7839(4) 0.0647(14) Uani 1 1 d . A 1 H2 H 0.5987 1.0345 0.8654 0.078 Uiso 1 1 calc R A 1 C3 C 0.4913(3) 0.9400(3) 0.7582(3) 0.0346(9) Uani 1 1 d . A 1 C4 C 0.5810(3) 1.1385(3) 0.7690(4) 0.0568(12) Uani 1 1 d . A 1 H4A H 0.6478 1.1822 0.8074 0.085 Uiso 1 1 calc R A 1 H4B H 0.5089 1.1676 0.7987 0.085 Uiso 1 1 calc R A 1 H4C H 0.5810 1.1423 0.6908 0.085 Uiso 1 1 calc R A 1 C5 C 0.4006(4) 0.9447(3) 0.8387(4) 0.0605(13) Uani 1 1 d . A 1 H5A H 0.4354 0.9332 0.9092 0.091 Uiso 1 1 calc R A 1 H5B H 0.3401 0.8872 0.8130 0.091 Uiso 1 1 calc R A 1 H5C H 0.3661 1.0166 0.8475 0.091 Uiso 1 1 calc R A 1 C6 C 0.4303(4) 0.9539(4) 0.6494(3) 0.0792(17) Uani 1 1 d . A 1 H6A H 0.3838 1.0192 0.6607 0.119 Uiso 1 1 calc R A 1 H6B H 0.3794 0.8891 0.6217 0.119 Uiso 1 1 calc R A 1 H6C H 0.4888 0.9623 0.5961 0.119 Uiso 1 1 calc R A 1 C7 C 0.8056(3) 1.0194(2) 0.7529(2) 0.0202(7) Uani 1 1 d . A 1 C8 C 0.8671(3) 1.0567(2) 0.8544(2) 0.0219(7) Uani 1 1 d . A 1 C9 C 0.9771(3) 1.1027(2) 0.8532(3) 0.0261(8) Uani 1 1 d . A 1 H9 H 1.0193 1.1267 0.9211 0.031 Uiso 1 1 calc R A 1 C10 C 1.0296(3) 1.1157(2) 0.7576(3) 0.0257(8) Uani 1 1 d . A 1 C11 C 0.9661(3) 1.0832(2) 0.6588(3) 0.0256(8) Uani 1 1 d . A 1 H11 H 1.0005 1.0911 0.5923 0.031 Uiso 1 1 calc R A 1 C12 C 0.8529(3) 1.0393(2) 0.6557(2) 0.0197(7) Uani 1 1 d . A 1 C13 C 0.8142(3) 1.0502(3) 0.9625(2) 0.0313(9) Uani 1 1 d . A 1 H13A H 0.8760 1.0430 1.0175 0.047 Uiso 1 1 calc R A 1 H13B H 0.7597 0.9863 0.9537 0.047 Uiso 1 1 calc R A 1 H13C H 0.7726 1.1170 0.9864 0.047 Uiso 1 1 calc R A 1 C14 C 1.1507(3) 1.1653(3) 0.7622(3) 0.0390(9) Uani 1 1 d . A 1 H14A H 1.1570 1.2329 0.8163 0.059 Uiso 1 1 calc R A 1 H14B H 1.1681 1.1820 0.6901 0.059 Uiso 1 1 calc R A 1 H14C H 1.2061 1.1133 0.7830 0.059 Uiso 1 1 calc R A 1 C15 C 0.7823(3) 1.0230(3) 0.5472(2) 0.0327(9) Uani 1 1 d . A 1 H15A H 0.7191 0.9680 0.5477 0.049 Uiso 1 1 calc R A 1 H15B H 0.8328 0.9979 0.4874 0.049 Uiso 1 1 calc R A 1 H15C H 0.7495 1.0926 0.5366 0.049 Uiso 1 1 calc R A 1 C16 C 0.5029(3) 0.7317(2) 0.7424(3) 0.0242(8) Uani 1 1 d . A 1 C17 C 0.5022(3) 0.6888(3) 0.8393(3) 0.0260(8) Uani 1 1 d . A 1 C18 C 0.4516(3) 0.5840(3) 0.8378(3) 0.0321(9) Uani 1 1 d . A 1 H18 H 0.4501 0.5551 0.9039 0.039 Uiso 1 1 calc R A 1 C19 C 0.4037(3) 0.5218(3) 0.7419(3) 0.0332(9) Uani 1 1 d . A 1 C20 C 0.4082(3) 0.5649(3) 0.6467(3) 0.0323(9) Uani 1 1 d . A 1 H20 H 0.3760 0.5220 0.5806 0.039 Uiso 1 1 calc R A 1 C21 C 0.4577(3) 0.6683(3) 0.6430(3) 0.0249(8) Uani 1 1 d . A 1 C22 C 0.5636(3) 0.7491(3) 0.9453(2) 0.0350(9) Uani 1 1 d . A 1 H22A H 0.6442 0.7686 0.9316 0.052 Uiso 1 1 calc R A 1 H22B H 0.5631 0.7014 1.0007 0.052 Uiso 1 1 calc R A 1 H22C H 0.5230 0.8159 0.9715 0.052 Uiso 1 1 calc R A 1 C23 C 0.3501(3) 0.4086(3) 0.7432(3) 0.0492(11) Uani 1 1 d . A 1 H23A H 0.2738 0.4153 0.7749 0.074 Uiso 1 1 calc R A 1 H23B H 0.4009 0.3692 0.7873 0.074 Uiso 1 1 calc R A 1 H23C H 0.3409 0.3679 0.6682 0.074 Uiso 1 1 calc R A 1 C24 C 0.4681(3) 0.7047(3) 0.5336(2) 0.0343(9) Uani 1 1 d . A 1 H24A H 0.4802 0.6409 0.4774 0.051 Uiso 1 1 calc R A 1 H24B H 0.5343 0.7575 0.5378 0.051 Uiso 1 1 calc R A 1 H24C H 0.3965 0.7393 0.5145 0.051 Uiso 1 1 calc R A 1 C25 C 0.7405(3) 0.6229(2) 0.7004(2) 0.0264(8) Uani 1 1 d . A 1 H25 H 0.6608 0.6122 0.7141 0.032 Uiso 1 1 calc R A 1 C26 C 0.8145(3) 0.5311(2) 0.6769(2) 0.0235(8) Uani 1 1 d . A 1 C27 C 0.7719(3) 0.4225(3) 0.6698(3) 0.0319(9) Uani 1 1 d . A 1 H27 H 0.6925 0.4081 0.6820 0.038 Uiso 1 1 calc R A 1 C28 C 0.8438(3) 0.3371(3) 0.6453(3) 0.0374(9) Uani 1 1 d . A 1 H28 H 0.8143 0.2638 0.6413 0.045 Uiso 1 1 calc R A 1 C29 C 0.9607(3) 0.3576(3) 0.6261(3) 0.0348(9) Uani 1 1 d . A 1 H29 H 1.0104 0.2981 0.6099 0.042 Uiso 1 1 calc R A 1 C30 C 1.0048(3) 0.4646(3) 0.6306(2) 0.0286(8) Uani 1 1 d . A 1 H30 H 1.0833 0.4788 0.6149 0.034 Uiso 1 1 calc R A 1 C31 C 0.9314(3) 0.5494(3) 0.6584(2) 0.0251(8) Uani 1 1 d . A 1 C32 C 1.0861(3) 0.6953(3) 0.6711(3) 0.0290(8) Uani 1 1 d . A 1 H32 H 1.1251 0.6518 0.6087 0.035 Uiso 1 1 calc R A 1 C33 C 1.0864(3) 0.8133(3) 0.6573(3) 0.0365(9) Uani 1 1 d . A 1 H33A H 1.0410 0.8198 0.5902 0.055 Uiso 1 1 calc R A 1 H33B H 1.1666 0.8405 0.6525 0.055 Uiso 1 1 calc R A 1 H33C H 1.0518 0.8567 0.7203 0.055 Uiso 1 1 calc R A 1 C34 C 1.1446(3) 0.6783(3) 0.7776(3) 0.0354(9) Uani 1 1 d . A 1 H34A H 1.1111 0.7259 0.8384 0.053 Uiso 1 1 calc R A 1 H34B H 1.2281 0.6964 0.7774 0.053 Uiso 1 1 calc R A 1 H34C H 1.1327 0.6015 0.7861 0.053 Uiso 1 1 calc R A 1 C41 C 0.9615(7) 0.4542(5) 0.9716(4) 0.115(3) Uani 1 1 d . . 3 H41A H 0.9734 0.3884 1.0056 0.138 Uiso 1 1 calc R . 3 H41B H 0.9811 0.4364 0.8939 0.138 Uiso 1 1 calc R . 3 C42 C 0.8323(8) 0.4854(7) 0.9783(5) 0.136(3) Uani 1 1 d . B 3 H42A H 0.8147 0.5160 1.0544 0.163 Uiso 1 1 calc R B 3 H42B H 0.8143 0.5400 0.9308 0.163 Uiso 1 1 calc R B 3 C43 C 0.7714(12) 0.3904(12) 0.9430(9) 0.109(5) Uani 0.50 1 d P B 3 H43A H 0.7995 0.3555 0.8728 0.163 Uiso 0.50 1 calc PR B 3 H43B H 0.6887 0.4048 0.9337 0.163 Uiso 0.50 1 calc PR B 3 H43C H 0.7815 0.3415 0.9968 0.163 Uiso 0.50 1 calc PR B 3 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 0.0181(2) 0.01592(14) 0.01284(15) 0.00057(10) -0.00094(13) 0.00079(13) Cl1 0.0315(6) 0.0276(4) 0.0171(5) 0.0001(3) -0.0082(4) 0.0028(4) Cl2 0.0326(6) 0.0334(5) 0.0141(4) 0.0043(3) 0.0029(4) 0.0071(4) Cl2B 0.091(11) 0.098(11) 0.102(11) 0.028(8) -0.010(8) 0.021(8) Cl1B 0.065(13) 0.072(13) 0.125(18) -0.081(13) -0.014(12) -0.013(12) Ru2 0.033(4) 0.040(4) 0.130(8) -0.037(4) -0.023(5) 0.006(4) O1 0.0223(13) 0.0251(12) 0.0340(14) 0.0055(10) 0.0024(11) 0.0005(10) N1 0.0189(16) 0.0194(13) 0.0214(15) 0.0015(11) 0.0030(12) 0.0059(12) N2 0.0195(16) 0.0184(13) 0.0233(15) 0.0009(11) -0.0012(12) 0.0011(12) C1 0.029(2) 0.0214(15) 0.0070(15) -0.0010(12) -0.0096(14) -0.0004(15) C2 0.035(3) 0.032(2) 0.126(4) 0.009(3) 0.006(3) 0.004(2) C3 0.026(2) 0.0262(18) 0.049(2) -0.0027(16) 0.0046(19) 0.0063(17) C4 0.033(2) 0.029(2) 0.107(4) 0.008(2) 0.006(2) 0.0080(19) C5 0.062(3) 0.039(2) 0.082(3) 0.006(2) 0.032(3) 0.004(2) C6 0.104(4) 0.069(3) 0.056(3) -0.011(2) -0.037(3) 0.045(3) C7 0.0196(18) 0.0179(14) 0.0212(18) -0.0029(13) 0.0019(15) 0.0025(14) C8 0.028(2) 0.0181(15) 0.0196(18) 0.0018(13) 0.0004(15) 0.0046(14) C9 0.032(2) 0.0239(16) 0.0205(19) 0.0005(13) -0.0084(16) -0.0001(15) C10 0.025(2) 0.0218(16) 0.030(2) 0.0060(14) -0.0060(16) -0.0004(15) C11 0.032(2) 0.0237(16) 0.0219(18) 0.0062(13) -0.0009(16) -0.0008(15) C12 0.0242(19) 0.0179(14) 0.0163(17) 0.0012(12) -0.0030(14) 0.0032(14) C13 0.038(2) 0.0344(19) 0.0193(19) -0.0013(14) -0.0013(16) 0.0018(17) C14 0.035(2) 0.043(2) 0.037(2) 0.0107(17) -0.0111(18) -0.0114(18) C15 0.036(2) 0.0343(19) 0.027(2) 0.0079(15) -0.0086(17) -0.0083(17) C16 0.0200(19) 0.0231(16) 0.0272(19) -0.0021(14) 0.0011(15) -0.0006(14) C17 0.028(2) 0.0269(17) 0.0219(19) 0.0024(14) 0.0024(16) -0.0022(15) C18 0.036(2) 0.0327(19) 0.029(2) 0.0098(15) 0.0036(17) -0.0027(17) C19 0.032(2) 0.0247(17) 0.041(2) 0.0013(16) 0.0040(18) -0.0053(16) C20 0.027(2) 0.0325(19) 0.032(2) -0.0064(16) -0.0045(17) -0.0015(17) C21 0.0198(19) 0.0283(17) 0.0255(19) 0.0012(14) -0.0008(15) 0.0035(15) C22 0.051(3) 0.0316(18) 0.0212(19) 0.0045(14) -0.0065(17) -0.0091(18) C23 0.054(3) 0.034(2) 0.056(3) 0.0005(19) 0.002(2) -0.012(2) C24 0.040(2) 0.0356(19) 0.024(2) -0.0036(15) -0.0013(17) 0.0027(18) C25 0.029(2) 0.0231(16) 0.0243(19) -0.0029(13) -0.0028(15) 0.0000(15) C26 0.028(2) 0.0245(17) 0.0184(17) 0.0035(13) 0.0009(15) 0.0051(15) C27 0.033(2) 0.0273(18) 0.035(2) 0.0045(15) 0.0005(17) -0.0026(17) C28 0.044(3) 0.0229(17) 0.043(2) 0.0014(16) -0.0016(19) -0.0012(18) C29 0.040(2) 0.0282(18) 0.035(2) -0.0006(15) 0.0031(18) 0.0080(18) C30 0.030(2) 0.0304(18) 0.0250(19) 0.0017(14) 0.0023(16) 0.0059(16) C31 0.032(2) 0.0230(16) 0.0205(18) 0.0061(13) -0.0015(16) 0.0015(16) C32 0.020(2) 0.0339(19) 0.034(2) 0.0098(16) -0.0009(17) 0.0006(16) C33 0.030(2) 0.033(2) 0.047(2) 0.0117(17) -0.0014(18) -0.0048(17) C34 0.032(2) 0.0339(19) 0.040(2) 0.0072(16) -0.0033(18) -0.0015(17) C41 0.181(9) 0.114(6) 0.069(5) 0.044(4) 0.070(5) 0.042(6) C42 0.207(10) 0.161(8) 0.055(4) 0.044(5) 0.046(5) 0.056(7) C43 0.130(12) 0.147(13) 0.049(8) 0.018(8) 0.007(7) -0.008(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 C25 1.840(3) . yes Ru1 C1 1.969(3) . yes Ru1 O1 2.255(2) . yes Ru1 Cl1 2.3288(8) . yes Ru1 Cl2 2.3446(8) . yes Cl2B Ru2 2.36(3) . yes Cl1B Ru2 2.33(2) . yes O1 C31 1.376(3) . ? O1 C32 1.479(4) . ? N1 C1 1.373(4) . ? N1 C7 1.427(4) . ? N1 C2 1.457(4) . ? N2 C1 1.368(4) . ? N2 C16 1.433(4) . ? N2 C3 1.488(4) . ? C2 C4 1.438(5) . ? C2 C3 1.509(5) . ? C3 C5 1.474(5) . ? C3 C6 1.532(5) . ? C7 C12 1.402(4) . ? C7 C8 1.415(4) . ? C8 C9 1.371(4) . ? C8 C13 1.513(4) . ? C9 C10 1.387(4) . ? C10 C11 1.390(4) . ? C10 C14 1.499(4) . ? C11 C12 1.390(4) . ? C12 C15 1.521(4) . ? C16 C17 1.394(4) . ? C16 C21 1.413(4) . ? C17 C18 1.400(4) . ? C17 C22 1.528(4) . ? C18 C19 1.383(4) . ? C19 C20 1.379(4) . ? C19 C23 1.514(4) . ? C20 C21 1.391(4) . ? C21 C24 1.510(4) . ? C25 C26 1.444(4) . ? C26 C31 1.394(4) . ? C26 C27 1.401(4) . ? C27 C28 1.369(4) . ? C28 C29 1.400(5) . ? C29 C30 1.393(4) . ? C30 C31 1.380(4) . ? C32 C33 1.499(4) . ? C32 C34 1.506(4) . ? C41 C41 1.473(12) 2_767 ? C41 C42 1.554(9) . ? C42 C43 1.344(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 C25 Ru1 C1 103.09(14) . . yes C25 Ru1 O1 79.52(12) . . yes C1 Ru1 O1 177.38(11) . . yes C25 Ru1 Cl1 98.12(10) . . yes C1 Ru1 Cl1 93.31(8) . . yes O1 Ru1 Cl1 86.49(6) . . yes C25 Ru1 Cl2 96.93(9) . . yes C1 Ru1 Cl2 94.09(8) . . yes O1 Ru1 Cl2 85.34(6) . . yes Cl1 Ru1 Cl2 161.26(4) . . yes Cl1B Ru2 Cl2B 160.3(10) . . yes C31 O1 C32 119.9(2) . . ? C31 O1 Ru1 110.35(19) . . ? C32 O1 Ru1 128.72(18) . . ? C1 N1 C7 122.4(3) . . ? C1 N1 C2 112.5(3) . . ? C7 N1 C2 123.9(3) . . ? C1 N2 C16 124.1(2) . . ? C1 N2 C3 113.3(3) . . ? C16 N2 C3 122.6(3) . . ? N2 C1 N1 106.1(3) . . ? N2 C1 Ru1 134.4(2) . . ? N1 C1 Ru1 119.5(2) . . ? C4 C2 N1 118.7(3) . . ? C4 C2 C3 124.9(4) . . ? N1 C2 C3 104.1(3) . . ? C5 C3 N2 115.0(3) . . ? C5 C3 C2 116.0(3) . . ? N2 C3 C2 101.2(3) . . ? C5 C3 C6 106.7(4) . . ? N2 C3 C6 110.0(3) . . ? C2 C3 C6 107.7(4) . . ? C12 C7 C8 119.8(3) . . ? C12 C7 N1 119.6(3) . . ? C8 C7 N1 120.4(3) . . ? C9 C8 C7 118.1(3) . . ? C9 C8 C13 119.8(3) . . ? C7 C8 C13 122.1(3) . . ? C8 C9 C10 123.1(3) . . ? C9 C10 C11 118.1(3) . . ? C9 C10 C14 120.4(3) . . ? C11 C10 C14 121.5(3) . . ? C10 C11 C12 121.0(3) . . ? C11 C12 C7 119.4(3) . . ? C11 C12 C15 117.9(3) . . ? C7 C12 C15 122.6(3) . . ? C17 C16 C21 120.4(3) . . ? C17 C16 N2 119.3(3) . . ? C21 C16 N2 120.2(3) . . ? C16 C17 C18 119.3(3) . . ? C16 C17 C22 121.8(3) . . ? C18 C17 C22 118.8(3) . . ? C19 C18 C17 121.3(3) . . ? C20 C19 C18 118.3(3) . . ? C20 C19 C23 121.8(3) . . ? C18 C19 C23 119.9(3) . . ? C19 C20 C21 123.0(3) . . ? C20 C21 C16 117.7(3) . . ? C20 C21 C24 119.3(3) . . ? C16 C21 C24 122.9(3) . . ? C26 C25 Ru1 117.8(2) . . ? C31 C26 C27 118.3(3) . . ? C31 C26 C25 119.8(3) . . ? C27 C26 C25 121.9(3) . . ? C28 C27 C26 120.5(3) . . ? C27 C28 C29 120.1(3) . . ? C30 C29 C28 120.5(3) . . ? C31 C30 C29 118.3(3) . . ? O1 C31 C30 125.2(3) . . ? O1 C31 C26 112.6(3) . . ? C30 C31 C26 122.2(3) . . ? O1 C32 C33 105.3(3) . . ? O1 C32 C34 109.9(3) . . ? C33 C32 C34 113.3(3) . . ? C41 C41 C42 110.2(8) 2_767 . ? C43 C42 C41 104.3(9) . . ? _diffrn_measured_fraction_theta_max 0.832 _diffrn_reflns_theta_full 31.98 _diffrn_measured_fraction_theta_full 0.832 _refine_diff_density_max 2.037 _refine_diff_density_min -1.337 _refine_diff_density_rms 0.125;