# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- andyg- chem sci.cif' _publ_contact_author ; Peter G. Jones Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; _publ_contact_author_phone '049 531 391-5382' _publ_contact_author_fax '049 531 391-5387' _publ_contact_author_email p.jones@tu-bs.de #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Facile \h7-\h3 hapticity interconversion in pentamethylcyclopentadienyl ruthenium(II) complexes containing a phenylmethallyl (open indenyl) ligand. ; loop_ _publ_author_name _publ_author_address A.Glockner ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; O.Arias ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; T.Bannenberg ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; C.G.Daniliuc ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; P.G.Jones ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; M.Tamm ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; _publ_contact_author_name 'Peter G. Jones' #============================================================================= # cif data for "andyg29" (compound 1) #============================================================================= data_andyg29 _database_code_depnum_ccdc_archive 'CCDC 832071' #TrackingRef '- andyg- chem sci.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H26 Ru' _chemical_formula_weight 367.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 13.4601(2) _cell_length_b 7.11350(10) _cell_length_c 17.8388(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.424(2) _cell_angle_gamma 90.00 _cell_volume 1654.20(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15580 _cell_measurement_theta_min 3.3876 _cell_measurement_theta_max 75.6369 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 7.572 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.43688 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20622 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 75.82 _reflns_number_total 3419 _reflns_number_gt 3221 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _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^)+(0.0522P)^2^+2.7797P] 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 ; The hydrogens of the C1, C3 and c5 atoms were refined freely. The methyls were refined using a rigid model, others riding. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3419 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 Ru Ru 0.777931(16) 0.89210(3) 0.110159(11) 0.02169(10) Uani 1 1 d . . . C1 C 0.8807(3) 1.1165(4) 0.0901(2) 0.0305(7) Uani 1 1 d . . . H1A H 0.943(3) 1.083(5) 0.070(2) 0.035(10) Uiso 1 1 d . . . H1B H 0.894(3) 1.222(6) 0.130(2) 0.049(12) Uiso 1 1 d . . . C2 C 0.7891(3) 1.1160(4) 0.02934(19) 0.0289(7) Uani 1 1 d . . . C3 C 0.6904(3) 1.1217(4) 0.04439(18) 0.0272(6) Uani 1 1 d . . . H3 H 0.633(3) 1.111(4) -0.001(2) 0.023(9) Uiso 1 1 d . . . C4 C 0.6668(3) 1.1160(4) 0.11890(19) 0.0269(6) Uani 1 1 d . . . C5 C 0.7448(3) 1.1251(4) 0.19099(19) 0.0281(6) Uani 1 1 d . . . H5 H 0.800(3) 1.199(5) 0.1965(19) 0.023(8) Uiso 1 1 d . . . C6 C 0.7146(3) 1.0852(5) 0.26068(19) 0.0338(7) Uani 1 1 d . . . H6 H 0.7653 1.0869 0.3085 0.041 Uiso 1 1 calc R . . C7 C 0.6156(3) 1.0446(5) 0.2611(2) 0.0389(8) Uani 1 1 d . . . H7 H 0.5983 1.0167 0.3083 0.047 Uiso 1 1 calc R . . C8 C 0.5388(3) 1.0443(5) 0.1905(2) 0.0361(7) Uani 1 1 d . . . H8 H 0.4695 1.0204 0.1910 0.043 Uiso 1 1 calc R . . C9 C 0.5625(3) 1.0775(5) 0.1224(2) 0.0324(7) Uani 1 1 d . . . H9 H 0.5096 1.0756 0.0758 0.039 Uiso 1 1 calc R . . C10 C 0.7933(3) 1.0877(5) -0.0537(2) 0.0396(8) Uani 1 1 d . . . H10A H 0.7345 1.0119 -0.0808 0.047 Uiso 1 1 calc R . . H10B H 0.8571 1.0227 -0.0550 0.047 Uiso 1 1 calc R . . H10C H 0.7912 1.2102 -0.0792 0.047 Uiso 1 1 calc R . . C11 C 0.8288(2) 0.6428(4) 0.06136(18) 0.0258(6) Uani 1 1 d . . . C12 C 0.7217(2) 0.6230(4) 0.05730(18) 0.0245(6) Uani 1 1 d . . . C13 C 0.7098(3) 0.6245(4) 0.13396(19) 0.0267(6) Uani 1 1 d . . . C14 C 0.8091(2) 0.6429(4) 0.18640(17) 0.0258(6) Uani 1 1 d . . . C15 C 0.8830(2) 0.6533(4) 0.14177(18) 0.0264(6) Uani 1 1 d . . . C16 C 0.8773(3) 0.6280(5) -0.0057(2) 0.0364(7) Uani 1 1 d . . . H16A H 0.8978 0.4975 -0.0110 0.044 Uiso 1 1 calc R . . H16B H 0.9378 0.7095 0.0035 0.044 Uiso 1 1 calc R . . H16C H 0.8278 0.6673 -0.0532 0.044 Uiso 1 1 calc R . . C17 C 0.6385(3) 0.5931(4) -0.01531(19) 0.0327(7) Uani 1 1 d . . . H17A H 0.6366 0.4602 -0.0301 0.039 Uiso 1 1 calc R . . H17B H 0.6524 0.6704 -0.0570 0.039 Uiso 1 1 calc R . . H17C H 0.5723 0.6292 -0.0062 0.039 Uiso 1 1 calc R . . C18 C 0.6116(3) 0.5935(4) 0.1583(2) 0.0336(7) Uani 1 1 d . . . H18A H 0.5532 0.6317 0.1163 0.040 Uiso 1 1 calc R . . H18B H 0.6127 0.6686 0.2046 0.040 Uiso 1 1 calc R . . H18C H 0.6051 0.4601 0.1699 0.040 Uiso 1 1 calc R . . C19 C 0.8305(3) 0.6368(5) 0.27288(19) 0.0351(7) Uani 1 1 d . . . H19A H 0.8297 0.5059 0.2899 0.042 Uiso 1 1 calc R . . H19B H 0.7778 0.7084 0.2898 0.042 Uiso 1 1 calc R . . H19C H 0.8980 0.6920 0.2955 0.042 Uiso 1 1 calc R . . C20 C 0.9972(3) 0.6593(5) 0.1724(2) 0.0392(8) Uani 1 1 d . . . H20A H 1.0145 0.7280 0.2216 0.047 Uiso 1 1 calc R . . H20B H 1.0280 0.7230 0.1350 0.047 Uiso 1 1 calc R . . H20C H 1.0240 0.5308 0.1807 0.047 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 Ru 0.02527(14) 0.01794(14) 0.02055(14) 0.00091(7) 0.00324(9) 0.00052(7) C1 0.0358(17) 0.0241(16) 0.0316(16) 0.0033(12) 0.0083(14) -0.0090(12) C2 0.0406(18) 0.0205(15) 0.0252(15) 0.0079(11) 0.0077(13) -0.0014(11) C3 0.0367(17) 0.0167(14) 0.0242(14) 0.0022(10) 0.0003(13) 0.0033(11) C4 0.0340(17) 0.0149(14) 0.0306(16) -0.0026(10) 0.0059(13) 0.0051(11) C5 0.0289(16) 0.0229(15) 0.0311(16) -0.0065(11) 0.0047(13) 0.0018(12) C6 0.0403(18) 0.0337(17) 0.0247(15) -0.0076(12) 0.0032(13) 0.0065(14) C7 0.047(2) 0.0382(19) 0.0351(17) -0.0021(15) 0.0174(15) 0.0046(16) C8 0.0318(16) 0.0317(17) 0.0471(19) -0.0042(15) 0.0141(14) 0.0027(13) C9 0.0281(15) 0.0278(15) 0.0383(17) -0.0056(13) 0.0024(13) 0.0061(12) C10 0.057(2) 0.0338(18) 0.0294(17) 0.0054(13) 0.0146(16) -0.0008(15) C11 0.0315(15) 0.0173(13) 0.0295(15) 0.0014(11) 0.0092(12) 0.0056(11) C12 0.0276(15) 0.0169(13) 0.0270(15) -0.0002(10) 0.0031(12) 0.0019(10) C13 0.0322(16) 0.0166(13) 0.0314(16) 0.0015(11) 0.0082(13) -0.0023(11) C14 0.0354(16) 0.0172(13) 0.0230(14) 0.0037(11) 0.0035(12) 0.0030(11) C15 0.0288(15) 0.0168(13) 0.0313(15) 0.0035(11) 0.0033(12) 0.0032(11) C16 0.045(2) 0.0323(17) 0.0365(17) 0.0016(13) 0.0185(15) 0.0051(14) C17 0.0374(18) 0.0247(16) 0.0300(16) -0.0001(12) -0.0032(13) 0.0016(12) C18 0.0356(18) 0.0253(16) 0.0431(19) -0.0008(13) 0.0159(15) -0.0019(12) C19 0.052(2) 0.0279(16) 0.0238(15) 0.0019(12) 0.0057(14) 0.0008(14) C20 0.0272(16) 0.0367(18) 0.049(2) 0.0058(16) 0.0004(14) 0.0003(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C11 2.161(3) . ? Ru C3 2.178(3) . ? Ru C2 2.179(3) . ? Ru C12 2.184(3) . ? Ru C15 2.192(3) . ? Ru C1 2.199(3) . ? Ru C13 2.200(3) . ? Ru C14 2.210(3) . ? Ru C4 2.216(3) . ? Ru C5 2.312(3) . ? C1 C2 1.425(5) . ? C2 C3 1.420(5) . ? C2 C10 1.510(5) . ? C3 C4 1.442(5) . ? C4 C5 1.445(5) . ? C4 C9 1.447(5) . ? C5 C6 1.430(5) . ? C6 C7 1.365(5) . ? C7 C8 1.416(5) . ? C8 C9 1.351(5) . ? C11 C12 1.432(4) . ? C11 C15 1.440(4) . ? C11 C16 1.501(4) . ? C12 C13 1.416(4) . ? C12 C17 1.501(4) . ? C13 C14 1.433(4) . ? C13 C18 1.507(5) . ? C14 C15 1.422(4) . ? C14 C19 1.498(4) . ? C15 C20 1.499(4) . ? 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 C11 Ru C3 125.57(12) . . ? C11 Ru C2 104.63(12) . . ? C3 Ru C2 38.05(13) . . ? C11 Ru C12 38.49(12) . . ? C3 Ru C12 109.99(11) . . ? C2 Ru C12 115.38(12) . . ? C11 Ru C15 38.62(11) . . ? C3 Ru C15 161.33(12) . . ? C2 Ru C15 126.19(12) . . ? C12 Ru C15 64.14(11) . . ? C11 Ru C1 104.77(13) . . ? C3 Ru C1 69.27(13) . . ? C2 Ru C1 37.98(13) . . ? C12 Ru C1 136.92(13) . . ? C15 Ru C1 102.29(13) . . ? C11 Ru C13 63.67(12) . . ? C3 Ru C13 123.87(12) . . ? C2 Ru C13 149.46(12) . . ? C12 Ru C13 37.68(12) . . ? C15 Ru C13 63.43(12) . . ? C1 Ru C13 165.67(13) . . ? C11 Ru C14 63.83(11) . . ? C3 Ru C14 158.01(13) . . ? C2 Ru C14 163.73(13) . . ? C12 Ru C14 63.57(11) . . ? C15 Ru C14 37.69(12) . . ? C1 Ru C14 130.67(12) . . ? C13 Ru C14 37.94(12) . . ? C11 Ru C4 154.85(12) . . ? C3 Ru C4 38.29(12) . . ? C2 Ru C4 71.34(12) . . ? C12 Ru C4 119.53(12) . . ? C15 Ru C4 160.37(12) . . ? C1 Ru C4 87.28(13) . . ? C13 Ru C4 106.71(12) . . ? C14 Ru C4 124.13(12) . . ? C11 Ru C5 165.77(12) . . ? C3 Ru C5 68.65(11) . . ? C2 Ru C5 86.81(13) . . ? C12 Ru C5 142.92(12) . . ? C15 Ru C5 127.39(12) . . ? C1 Ru C5 78.91(13) . . ? C13 Ru C5 110.23(12) . . ? C14 Ru C5 103.17(12) . . ? C4 Ru C5 37.13(12) . . ? C2 C1 Ru 70.24(17) . . ? C3 C2 C1 121.9(3) . . ? C3 C2 C10 117.1(3) . . ? C1 C2 C10 120.7(3) . . ? C3 C2 Ru 70.95(17) . . ? C1 C2 Ru 71.78(17) . . ? C10 C2 Ru 125.3(2) . . ? C2 C3 C4 127.2(3) . . ? C2 C3 Ru 71.00(17) . . ? C4 C3 Ru 72.30(16) . . ? C3 C4 C5 122.8(3) . . ? C3 C4 C9 118.9(3) . . ? C5 C4 C9 117.9(3) . . ? C3 C4 Ru 69.41(17) . . ? C5 C4 Ru 75.04(17) . . ? C9 C4 Ru 123.1(2) . . ? C6 C5 C4 117.6(3) . . ? C6 C5 Ru 122.7(2) . . ? C4 C5 Ru 67.83(16) . . ? C7 C6 C5 122.4(3) . . ? C6 C7 C8 119.5(3) . . ? C9 C8 C7 121.1(3) . . ? C8 C9 C4 121.4(3) . . ? C12 C11 C15 108.0(3) . . ? C12 C11 C16 125.7(3) . . ? C15 C11 C16 125.8(3) . . ? C12 C11 Ru 71.64(16) . . ? C15 C11 Ru 71.86(17) . . ? C16 C11 Ru 128.5(2) . . ? C13 C12 C11 107.7(3) . . ? C13 C12 C17 126.5(3) . . ? C11 C12 C17 125.6(3) . . ? C13 C12 Ru 71.74(16) . . ? C11 C12 Ru 69.87(16) . . ? C17 C12 Ru 126.9(2) . . ? C12 C13 C14 108.7(3) . . ? C12 C13 C18 126.5(3) . . ? C14 C13 C18 124.6(3) . . ? C12 C13 Ru 70.58(16) . . ? C14 C13 Ru 71.43(17) . . ? C18 C13 Ru 128.3(2) . . ? C15 C14 C13 107.9(3) . . ? C15 C14 C19 126.6(3) . . ? C13 C14 C19 125.3(3) . . ? C15 C14 Ru 70.47(16) . . ? C13 C14 Ru 70.64(16) . . ? C19 C14 Ru 128.0(2) . . ? C14 C15 C11 107.7(3) . . ? C14 C15 C20 126.5(3) . . ? C11 C15 C20 125.7(3) . . ? C14 C15 Ru 71.84(17) . . ? C11 C15 Ru 69.52(16) . . ? C20 C15 Ru 127.5(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Ru C1 C2 95.0(2) . . . . ? C3 Ru C1 C2 -27.95(19) . . . . ? C12 Ru C1 C2 69.5(3) . . . . ? C15 Ru C1 C2 134.7(2) . . . . ? C13 Ru C1 C2 129.8(5) . . . . ? C14 Ru C1 C2 162.95(19) . . . . ? C4 Ru C1 C2 -62.6(2) . . . . ? C5 Ru C1 C2 -99.1(2) . . . . ? Ru C1 C2 C3 52.4(2) . . . . ? Ru C1 C2 C10 -120.8(3) . . . . ? C11 Ru C2 C3 129.94(18) . . . . ? C12 Ru C2 C3 90.43(19) . . . . ? C15 Ru C2 C3 165.89(17) . . . . ? C1 Ru C2 C3 -134.7(3) . . . . ? C13 Ru C2 C3 67.3(3) . . . . ? C14 Ru C2 C3 172.8(4) . . . . ? C4 Ru C2 C3 -24.12(18) . . . . ? C5 Ru C2 C3 -58.65(18) . . . . ? C11 Ru C2 C1 -95.4(2) . . . . ? C3 Ru C2 C1 134.7(3) . . . . ? C12 Ru C2 C1 -134.9(2) . . . . ? C15 Ru C2 C1 -59.4(2) . . . . ? C13 Ru C2 C1 -158.0(2) . . . . ? C14 Ru C2 C1 -52.5(5) . . . . ? C4 Ru C2 C1 110.5(2) . . . . ? C5 Ru C2 C1 76.0(2) . . . . ? C11 Ru C2 C10 19.7(3) . . . . ? C3 Ru C2 C10 -110.2(4) . . . . ? C12 Ru C2 C10 -19.8(4) . . . . ? C15 Ru C2 C10 55.7(4) . . . . ? C1 Ru C2 C10 115.1(4) . . . . ? C13 Ru C2 C10 -42.9(5) . . . . ? C14 Ru C2 C10 62.6(6) . . . . ? C4 Ru C2 C10 -134.3(3) . . . . ? C5 Ru C2 C10 -168.8(3) . . . . ? C1 C2 C3 C4 -4.4(5) . . . . ? C10 C2 C3 C4 169.0(3) . . . . ? Ru C2 C3 C4 48.3(3) . . . . ? C1 C2 C3 Ru -52.8(3) . . . . ? C10 C2 C3 Ru 120.6(3) . . . . ? C11 Ru C3 C2 -65.8(2) . . . . ? C12 Ru C3 C2 -105.99(19) . . . . ? C15 Ru C3 C2 -37.9(4) . . . . ? C1 Ru C3 C2 27.90(19) . . . . ? C13 Ru C3 C2 -145.62(18) . . . . ? C14 Ru C3 C2 -174.6(3) . . . . ? C4 Ru C3 C2 141.3(3) . . . . ? C5 Ru C3 C2 113.7(2) . . . . ? C11 Ru C3 C4 152.88(18) . . . . ? C2 Ru C3 C4 -141.3(3) . . . . ? C12 Ru C3 C4 112.69(19) . . . . ? C15 Ru C3 C4 -179.3(3) . . . . ? C1 Ru C3 C4 -113.4(2) . . . . ? C13 Ru C3 C4 73.1(2) . . . . ? C14 Ru C3 C4 44.1(4) . . . . ? C5 Ru C3 C4 -27.60(18) . . . . ? C2 C3 C4 C5 7.4(4) . . . . ? Ru C3 C4 C5 55.2(2) . . . . ? C2 C3 C4 C9 -165.2(3) . . . . ? Ru C3 C4 C9 -117.3(3) . . . . ? C2 C3 C4 Ru -47.9(3) . . . . ? C11 Ru C4 C3 -60.7(3) . . . . ? C2 Ru C4 C3 23.99(18) . . . . ? C12 Ru C4 C3 -85.2(2) . . . . ? C15 Ru C4 C3 179.3(3) . . . . ? C1 Ru C4 C3 59.22(19) . . . . ? C13 Ru C4 C3 -123.98(19) . . . . ? C14 Ru C4 C3 -161.67(18) . . . . ? C5 Ru C4 C3 134.4(3) . . . . ? C11 Ru C4 C5 164.9(3) . . . . ? C3 Ru C4 C5 -134.4(3) . . . . ? C2 Ru C4 C5 -110.4(2) . . . . ? C12 Ru C4 C5 140.42(19) . . . . ? C15 Ru C4 C5 44.9(4) . . . . ? C1 Ru C4 C5 -75.2(2) . . . . ? C13 Ru C4 C5 101.6(2) . . . . ? C14 Ru C4 C5 64.0(2) . . . . ? C11 Ru C4 C9 51.1(4) . . . . ? C3 Ru C4 C9 111.8(3) . . . . ? C2 Ru C4 C9 135.8(3) . . . . ? C12 Ru C4 C9 26.6(3) . . . . ? C15 Ru C4 C9 -68.9(5) . . . . ? C1 Ru C4 C9 171.0(3) . . . . ? C13 Ru C4 C9 -12.2(3) . . . . ? C14 Ru C4 C9 -49.9(3) . . . . ? C5 Ru C4 C9 -113.8(4) . . . . ? C3 C4 C5 C6 -169.2(3) . . . . ? C9 C4 C5 C6 3.4(4) . . . . ? Ru C4 C5 C6 -116.5(3) . . . . ? C3 C4 C5 Ru -52.8(2) . . . . ? C9 C4 C5 Ru 119.9(3) . . . . ? C11 Ru C5 C6 -43.7(6) . . . . ? C3 Ru C5 C6 137.9(3) . . . . ? C2 Ru C5 C6 172.3(3) . . . . ? C12 Ru C5 C6 42.6(4) . . . . ? C15 Ru C5 C6 -53.1(3) . . . . ? C1 Ru C5 C6 -150.2(3) . . . . ? C13 Ru C5 C6 18.3(3) . . . . ? C14 Ru C5 C6 -20.7(3) . . . . ? C4 Ru C5 C6 109.5(4) . . . . ? C11 Ru C5 C4 -153.2(4) . . . . ? C3 Ru C5 C4 28.40(19) . . . . ? C2 Ru C5 C4 62.8(2) . . . . ? C12 Ru C5 C4 -66.9(3) . . . . ? C15 Ru C5 C4 -162.63(18) . . . . ? C1 Ru C5 C4 100.3(2) . . . . ? C13 Ru C5 C4 -91.2(2) . . . . ? C14 Ru C5 C4 -130.20(19) . . . . ? C4 C5 C6 C7 -1.8(5) . . . . ? Ru C5 C6 C7 -82.0(4) . . . . ? C5 C6 C7 C8 -1.0(5) . . . . ? C6 C7 C8 C9 2.2(5) . . . . ? C7 C8 C9 C4 -0.5(5) . . . . ? C3 C4 C9 C8 170.6(3) . . . . ? C5 C4 C9 C8 -2.4(4) . . . . ? Ru C4 C9 C8 87.4(4) . . . . ? C3 Ru C11 C12 -77.0(2) . . . . ? C2 Ru C11 C12 -112.56(19) . . . . ? C15 Ru C11 C12 116.8(3) . . . . ? C1 Ru C11 C12 -151.88(18) . . . . ? C13 Ru C11 C12 37.20(18) . . . . ? C14 Ru C11 C12 79.70(19) . . . . ? C4 Ru C11 C12 -35.4(4) . . . . ? C5 Ru C11 C12 104.8(5) . . . . ? C3 Ru C11 C15 166.14(18) . . . . ? C2 Ru C11 C15 130.62(19) . . . . ? C12 Ru C11 C15 -116.8(3) . . . . ? C1 Ru C11 C15 91.3(2) . . . . ? C13 Ru C11 C15 -79.62(19) . . . . ? C14 Ru C11 C15 -37.12(18) . . . . ? C4 Ru C11 C15 -152.2(3) . . . . ? C5 Ru C11 C15 -12.0(6) . . . . ? C3 Ru C11 C16 44.4(4) . . . . ? C2 Ru C11 C16 8.9(3) . . . . ? C12 Ru C11 C16 121.5(4) . . . . ? C15 Ru C11 C16 -121.7(4) . . . . ? C1 Ru C11 C16 -30.4(3) . . . . ? C13 Ru C11 C16 158.7(3) . . . . ? C14 Ru C11 C16 -158.8(3) . . . . ? C4 Ru C11 C16 86.1(4) . . . . ? C5 Ru C11 C16 -133.7(5) . . . . ? C15 C11 C12 C13 1.0(3) . . . . ? C16 C11 C12 C13 173.2(3) . . . . ? Ru C11 C12 C13 -62.1(2) . . . . ? C15 C11 C12 C17 -175.3(3) . . . . ? C16 C11 C12 C17 -3.1(5) . . . . ? Ru C11 C12 C17 121.6(3) . . . . ? C15 C11 C12 Ru 63.1(2) . . . . ? C16 C11 C12 Ru -124.7(3) . . . . ? C11 Ru C12 C13 117.6(3) . . . . ? C3 Ru C12 C13 -119.95(19) . . . . ? C2 Ru C12 C13 -160.94(19) . . . . ? C15 Ru C12 C13 79.3(2) . . . . ? C1 Ru C12 C13 159.4(2) . . . . ? C14 Ru C12 C13 37.13(18) . . . . ? C4 Ru C12 C13 -78.9(2) . . . . ? C5 Ru C12 C13 -39.2(3) . . . . ? C3 Ru C12 C11 122.49(18) . . . . ? C2 Ru C12 C11 81.5(2) . . . . ? C15 Ru C12 C11 -38.25(17) . . . . ? C1 Ru C12 C11 41.9(3) . . . . ? C13 Ru C12 C11 -117.6(3) . . . . ? C14 Ru C12 C11 -80.43(19) . . . . ? C4 Ru C12 C11 163.57(17) . . . . ? C5 Ru C12 C11 -156.8(2) . . . . ? C11 Ru C12 C17 -120.0(4) . . . . ? C3 Ru C12 C17 2.5(3) . . . . ? C2 Ru C12 C17 -38.5(3) . . . . ? C15 Ru C12 C17 -158.3(3) . . . . ? C1 Ru C12 C17 -78.2(3) . . . . ? C13 Ru C12 C17 122.4(4) . . . . ? C14 Ru C12 C17 159.5(3) . . . . ? C4 Ru C12 C17 43.5(3) . . . . ? C5 Ru C12 C17 83.2(3) . . . . ? C11 C12 C13 C14 -0.7(3) . . . . ? C17 C12 C13 C14 175.6(3) . . . . ? Ru C12 C13 C14 -61.6(2) . . . . ? C11 C12 C13 C18 -175.2(3) . . . . ? C17 C12 C13 C18 1.0(5) . . . . ? Ru C12 C13 C18 123.8(3) . . . . ? C11 C12 C13 Ru 60.9(2) . . . . ? C17 C12 C13 Ru -122.8(3) . . . . ? C11 Ru C13 C12 -38.00(18) . . . . ? C3 Ru C13 C12 78.7(2) . . . . ? C2 Ru C13 C12 35.5(3) . . . . ? C15 Ru C13 C12 -81.3(2) . . . . ? C1 Ru C13 C12 -76.1(5) . . . . ? C14 Ru C13 C12 -118.5(3) . . . . ? C4 Ru C13 C12 116.95(19) . . . . ? C5 Ru C13 C12 156.01(18) . . . . ? C11 Ru C13 C14 80.46(19) . . . . ? C3 Ru C13 C14 -162.83(18) . . . . ? C2 Ru C13 C14 154.0(2) . . . . ? C12 Ru C13 C14 118.5(3) . . . . ? C15 Ru C13 C14 37.11(18) . . . . ? C1 Ru C13 C14 42.4(6) . . . . ? C4 Ru C13 C14 -124.59(18) . . . . ? C5 Ru C13 C14 -85.53(19) . . . . ? C11 Ru C13 C18 -159.7(3) . . . . ? C3 Ru C13 C18 -43.0(3) . . . . ? C2 Ru C13 C18 -86.2(4) . . . . ? C12 Ru C13 C18 -121.7(4) . . . . ? C15 Ru C13 C18 156.9(3) . . . . ? C1 Ru C13 C18 162.2(4) . . . . ? C14 Ru C13 C18 119.8(4) . . . . ? C4 Ru C13 C18 -4.8(3) . . . . ? C5 Ru C13 C18 34.3(3) . . . . ? C12 C13 C14 C15 0.1(3) . . . . ? C18 C13 C14 C15 174.8(3) . . . . ? Ru C13 C14 C15 -60.9(2) . . . . ? C12 C13 C14 C19 -175.5(3) . . . . ? C18 C13 C14 C19 -0.8(5) . . . . ? Ru C13 C14 C19 123.4(3) . . . . ? C12 C13 C14 Ru 61.1(2) . . . . ? C18 C13 C14 Ru -124.2(3) . . . . ? C11 Ru C14 C15 38.03(18) . . . . ? C3 Ru C14 C15 159.0(3) . . . . ? C2 Ru C14 C15 -9.1(5) . . . . ? C12 Ru C14 C15 81.18(19) . . . . ? C1 Ru C14 C15 -49.2(2) . . . . ? C13 Ru C14 C15 118.1(3) . . . . ? C4 Ru C14 C15 -169.67(17) . . . . ? C5 Ru C14 C15 -135.82(18) . . . . ? C11 Ru C14 C13 -80.0(2) . . . . ? C3 Ru C14 C13 40.9(4) . . . . ? C2 Ru C14 C13 -127.2(4) . . . . ? C12 Ru C14 C13 -36.88(18) . . . . ? C15 Ru C14 C13 -118.1(3) . . . . ? C1 Ru C14 C13 -167.29(19) . . . . ? C4 Ru C14 C13 72.3(2) . . . . ? C5 Ru C14 C13 106.12(19) . . . . ? C11 Ru C14 C19 159.7(3) . . . . ? C3 Ru C14 C19 -79.3(4) . . . . ? C2 Ru C14 C19 112.6(5) . . . . ? C12 Ru C14 C19 -157.1(3) . . . . ? C15 Ru C14 C19 121.7(4) . . . . ? C1 Ru C14 C19 72.5(3) . . . . ? C13 Ru C14 C19 -120.2(4) . . . . ? C4 Ru C14 C19 -48.0(3) . . . . ? C5 Ru C14 C19 -14.1(3) . . . . ? C13 C14 C15 C11 0.5(3) . . . . ? C19 C14 C15 C11 176.0(3) . . . . ? Ru C14 C15 C11 -60.6(2) . . . . ? C13 C14 C15 C20 -175.3(3) . . . . ? C19 C14 C15 C20 0.3(5) . . . . ? Ru C14 C15 C20 123.7(3) . . . . ? C13 C14 C15 Ru 61.0(2) . . . . ? C19 C14 C15 Ru -123.4(3) . . . . ? C12 C11 C15 C14 -0.9(3) . . . . ? C16 C11 C15 C14 -173.1(3) . . . . ? Ru C11 C15 C14 62.1(2) . . . . ? C12 C11 C15 C20 174.9(3) . . . . ? C16 C11 C15 C20 2.7(5) . . . . ? Ru C11 C15 C20 -122.2(3) . . . . ? C12 C11 C15 Ru -62.9(2) . . . . ? C16 C11 C15 Ru 124.8(3) . . . . ? C11 Ru C15 C14 -117.6(3) . . . . ? C3 Ru C15 C14 -155.2(3) . . . . ? C2 Ru C15 C14 176.84(18) . . . . ? C12 Ru C15 C14 -79.53(19) . . . . ? C1 Ru C15 C14 143.99(19) . . . . ? C13 Ru C15 C14 -37.34(18) . . . . ? C4 Ru C15 C14 26.2(4) . . . . ? C5 Ru C15 C14 58.7(2) . . . . ? C3 Ru C15 C11 -37.5(4) . . . . ? C2 Ru C15 C11 -65.5(2) . . . . ? C12 Ru C15 C11 38.11(18) . . . . ? C1 Ru C15 C11 -98.4(2) . . . . ? C13 Ru C15 C11 80.30(19) . . . . ? C14 Ru C15 C11 117.6(3) . . . . ? C4 Ru C15 C11 143.9(3) . . . . ? C5 Ru C15 C11 176.30(18) . . . . ? C11 Ru C15 C20 119.9(4) . . . . ? C3 Ru C15 C20 82.4(5) . . . . ? C2 Ru C15 C20 54.4(3) . . . . ? C12 Ru C15 C20 158.0(3) . . . . ? C1 Ru C15 C20 21.5(3) . . . . ? C13 Ru C15 C20 -159.8(3) . . . . ? C14 Ru C15 C20 -122.5(4) . . . . ? C4 Ru C15 C20 -96.2(4) . . . . ? C5 Ru C15 C20 -63.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 72.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.823 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.091 #============================================================================= # end of cif data for "andyg29" (compound 1) #============================================================================= #============================================================================= # cif data for "andyg31b" (compound 2-anti) #============================================================================= data_andyg31b _database_code_depnum_ccdc_archive 'CCDC 832072' #TrackingRef '- andyg- chem sci.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H35 P Ru' _chemical_formula_weight 443.55 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' 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 orthorhombic _symmetry_space_group_name_H-M 'P c c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 34.0568(14) _cell_length_b 14.0658(6) _cell_length_c 8.9452(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4285.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12990 _cell_measurement_theta_min 2.2722 _cell_measurement_theta_max 29.2369 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 0.810 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97014 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 108761 _diffrn_reflns_av_R_equivalents 0.1076 _diffrn_reflns_av_sigmaI/netI 0.0737 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4371 _reflns_number_gt 2923 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _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^)+(0.0000P)^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 ; The hydrogens of the C1 and C3 atoms were refined freely, but with C-H distance restraints (SADI). The methyls were refined using a rigid model, others riding. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4371 _refine_ls_number_parameters 246 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0265 _refine_ls_wR_factor_gt 0.0254 _refine_ls_goodness_of_fit_ref 0.849 _refine_ls_restrained_S_all 0.848 _refine_ls_shift/su_max 0.003 _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 Ru Ru 0.647702(5) 0.488051(10) 0.59263(2) 0.01009(4) Uani 1 1 d . . . P P 0.585855(17) 0.42862(4) 0.55173(7) 0.01363(15) Uani 1 1 d . . . C1 C 0.64205(8) 0.43805(16) 0.8230(3) 0.0164(6) Uani 1 1 d D . . H1A H 0.6611(5) 0.3959(11) 0.861(2) 0.015(6) Uiso 1 1 d D . . H1B H 0.6165(4) 0.4188(11) 0.839(2) 0.006(6) Uiso 1 1 d D . . C2 C 0.65256(7) 0.53570(14) 0.8169(2) 0.0159(6) Uani 1 1 d . . . C3 C 0.62663(7) 0.60129(14) 0.7435(3) 0.0135(6) Uani 1 1 d D . . H3 H 0.6380(5) 0.6575(10) 0.717(2) 0.016 Uiso 1 1 d D . . C4 C 0.58578(6) 0.61972(14) 0.7889(3) 0.0124(5) Uani 1 1 d U . . C5 C 0.57070(6) 0.58753(13) 0.9250(3) 0.0179(6) Uani 1 1 d . . . H5 H 0.5872 0.5524 0.9904 0.022 Uiso 1 1 calc R . . C6 C 0.53240(7) 0.60543(15) 0.9670(3) 0.0229(6) Uani 1 1 d . . . H6 H 0.5227 0.5812 1.0589 0.028 Uiso 1 1 calc R . . C7 C 0.50825(7) 0.65854(14) 0.8756(3) 0.0245(7) Uani 1 1 d . . . H7 H 0.4817 0.6700 0.9033 0.029 Uiso 1 1 calc R . . C8 C 0.52285(7) 0.69480(14) 0.7437(3) 0.0224(6) Uani 1 1 d . . . H8 H 0.5066 0.7329 0.6817 0.027 Uiso 1 1 calc R . . C9 C 0.56113(6) 0.67606(14) 0.7011(3) 0.0162(6) Uani 1 1 d . . . H9 H 0.5708 0.7020 0.6102 0.019 Uiso 1 1 calc R . . C10 C 0.69081(6) 0.56926(13) 0.8841(3) 0.0256(7) Uani 1 1 d . . . H10A H 0.6867 0.5860 0.9893 0.031 Uiso 1 1 calc R . . H10B H 0.7002 0.6252 0.8294 0.031 Uiso 1 1 calc R . . H10C H 0.7104 0.5184 0.8772 0.031 Uiso 1 1 calc R . . C11 C 0.70055(7) 0.55893(15) 0.5001(3) 0.0187(7) Uani 1 1 d . . . C12 C 0.71068(6) 0.46398(14) 0.5392(3) 0.0154(6) Uani 1 1 d . . . C13 C 0.68798(6) 0.40150(14) 0.4483(3) 0.0119(6) Uani 1 1 d . . . C14 C 0.66443(6) 0.45877(15) 0.3530(3) 0.0151(6) Uani 1 1 d . . . C15 C 0.67155(7) 0.55568(14) 0.3866(3) 0.0189(6) Uani 1 1 d . . . C16 C 0.72106(6) 0.64933(14) 0.5482(3) 0.0363(8) Uani 1 1 d . . . H16A H 0.7342 0.6781 0.4618 0.044 Uiso 1 1 calc R . . H16B H 0.7406 0.6344 0.6251 0.044 Uiso 1 1 calc R . . H16C H 0.7017 0.6940 0.5888 0.044 Uiso 1 1 calc R . . C17 C 0.74305(6) 0.43056(14) 0.6416(3) 0.0286(7) Uani 1 1 d . . . H17A H 0.7323 0.3858 0.7149 0.034 Uiso 1 1 calc R . . H17B H 0.7544 0.4853 0.6938 0.034 Uiso 1 1 calc R . . H17C H 0.7635 0.3989 0.5826 0.034 Uiso 1 1 calc R . . C18 C 0.69330(6) 0.29553(12) 0.4387(3) 0.0242(7) Uani 1 1 d . . . H18A H 0.7156 0.2811 0.3734 0.029 Uiso 1 1 calc R . . H18B H 0.6694 0.2666 0.3977 0.029 Uiso 1 1 calc R . . H18C H 0.6983 0.2699 0.5388 0.029 Uiso 1 1 calc R . . C19 C 0.64280(7) 0.42310(14) 0.2160(2) 0.0303(7) Uani 1 1 d . . . H19A H 0.6170 0.4538 0.2101 0.036 Uiso 1 1 calc R . . H19B H 0.6394 0.3541 0.2232 0.036 Uiso 1 1 calc R . . H19C H 0.6580 0.4383 0.1262 0.036 Uiso 1 1 calc R . . C20 C 0.65554(7) 0.64106(14) 0.3047(3) 0.0378(8) Uani 1 1 d . . . H20A H 0.6745 0.6616 0.2287 0.045 Uiso 1 1 calc R . . H20B H 0.6511 0.6929 0.3759 0.045 Uiso 1 1 calc R . . H20C H 0.6307 0.6242 0.2563 0.045 Uiso 1 1 calc R . . C21 C 0.58519(6) 0.30696(13) 0.4772(3) 0.0239(7) Uani 1 1 d . . . H21A H 0.5964 0.2633 0.5511 0.029 Uiso 1 1 calc R . . H21B H 0.6007 0.3044 0.3850 0.029 Uiso 1 1 calc R . . H21C H 0.5581 0.2883 0.4556 0.029 Uiso 1 1 calc R . . C22 C 0.54809(6) 0.41003(14) 0.6940(3) 0.0227(6) Uani 1 1 d . . . H22A H 0.5396 0.4716 0.7337 0.027 Uiso 1 1 calc R . . H22B H 0.5588 0.3712 0.7753 0.027 Uiso 1 1 calc R . . H22C H 0.5256 0.3773 0.6493 0.027 Uiso 1 1 calc R . . C23 C 0.55580(5) 0.49332(14) 0.4163(3) 0.0215(5) Uani 1 1 d . . . H23A H 0.5325 0.4556 0.3915 0.026 Uiso 1 1 calc R . . H23B H 0.5711 0.5048 0.3254 0.026 Uiso 1 1 calc R . . H23C H 0.5476 0.5542 0.4594 0.026 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 Ru 0.00861(7) 0.00943(8) 0.01223(9) -0.00004(9) 0.00021(11) 0.00007(9) P 0.0119(3) 0.0136(3) 0.0154(4) -0.0005(3) -0.0007(3) -0.0014(3) C1 0.0151(17) 0.0211(14) 0.0128(16) 0.0032(11) -0.0033(13) 0.0087(13) C2 0.0115(14) 0.0205(14) 0.0155(15) -0.0055(10) -0.0005(12) 0.0034(11) C3 0.0143(14) 0.0109(13) 0.0154(16) -0.0030(11) 0.0023(12) -0.0031(11) C4 0.0132(13) 0.0089(12) 0.0151(15) -0.0080(10) -0.0003(12) -0.0022(10) C5 0.0206(14) 0.0149(12) 0.0183(17) -0.0062(12) -0.0020(13) 0.0014(10) C6 0.0262(16) 0.0223(14) 0.0203(17) -0.0056(11) 0.0088(13) -0.0025(11) C7 0.0133(14) 0.0269(15) 0.033(2) -0.0119(13) 0.0078(13) 0.0038(11) C8 0.0191(15) 0.0182(14) 0.030(2) -0.0053(12) -0.0049(13) 0.0069(11) C9 0.0204(15) 0.0118(13) 0.0165(16) -0.0027(11) 0.0023(12) 0.0008(11) C10 0.0187(14) 0.0324(14) 0.0257(19) -0.0086(13) -0.0067(13) 0.0031(11) C11 0.0124(15) 0.0140(13) 0.0299(19) -0.0056(11) 0.0097(13) -0.0045(10) C12 0.0100(13) 0.0201(14) 0.0162(16) -0.0044(10) -0.0009(11) 0.0012(10) C13 0.0092(13) 0.0143(12) 0.0122(16) -0.0007(10) 0.0029(11) 0.0005(9) C14 0.0108(13) 0.0250(15) 0.0096(15) 0.0029(10) 0.0024(11) 0.0012(10) C15 0.0173(14) 0.0172(13) 0.0220(18) 0.0095(12) 0.0134(14) 0.0065(10) C16 0.0296(17) 0.0219(14) 0.058(2) -0.0175(14) 0.0228(15) -0.0123(11) C17 0.0106(15) 0.0394(15) 0.036(2) -0.0100(13) -0.0027(13) 0.0061(12) C18 0.0192(14) 0.0186(13) 0.035(2) -0.0057(12) 0.0064(13) 0.0029(10) C19 0.0289(16) 0.0455(16) 0.0167(16) 0.0003(13) 0.0019(14) 0.0067(14) C20 0.043(2) 0.0309(15) 0.040(2) 0.0189(13) 0.0228(16) 0.0161(13) C21 0.0138(14) 0.0218(14) 0.0361(19) -0.0052(12) 0.0005(13) -0.0027(11) C22 0.0144(15) 0.0264(15) 0.0272(18) -0.0023(13) 0.0036(12) -0.0076(11) C23 0.0130(10) 0.0243(12) 0.0271(14) -0.0001(15) -0.0045(12) 0.0016(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 Ru C2 2.122(2) . ? Ru C1 2.186(2) . ? Ru C3 2.208(2) . ? Ru C11 2.218(2) . ? Ru C12 2.223(2) . ? Ru C15 2.228(2) . ? Ru C13 2.243(2) . ? Ru C14 2.256(2) . ? Ru P 2.2955(6) . ? P C22 1.828(2) . ? P C23 1.828(2) . ? P C21 1.8367(18) . ? C1 C2 1.421(3) . ? C2 C3 1.436(3) . ? C2 C10 1.510(3) . ? C3 C4 1.472(3) . ? C4 C9 1.397(3) . ? C4 C5 1.397(3) . ? C5 C6 1.380(3) . ? C6 C7 1.380(3) . ? C7 C8 1.378(3) . ? C8 C9 1.383(3) . ? C11 C15 1.417(3) . ? C11 C12 1.423(3) . ? C11 C16 1.513(3) . ? C12 C13 1.425(3) . ? C12 C17 1.508(3) . ? C13 C14 1.421(3) . ? C13 C18 1.504(2) . ? C14 C15 1.417(3) . ? C14 C19 1.515(3) . ? C15 C20 1.509(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Ru C1 38.47(7) . . ? C2 Ru C3 38.68(7) . . ? C1 Ru C3 68.11(8) . . ? C2 Ru C11 98.48(9) . . ? C1 Ru C11 124.60(10) . . ? C3 Ru C11 99.64(8) . . ? C2 Ru C12 100.14(9) . . ? C1 Ru C12 103.80(9) . . ? C3 Ru C12 123.69(8) . . ? C11 Ru C12 37.38(7) . . ? C2 Ru C15 128.25(9) . . ? C1 Ru C15 161.72(10) . . ? C3 Ru C15 108.44(8) . . ? C11 Ru C15 37.19(8) . . ? C12 Ru C15 62.32(8) . . ? C2 Ru C13 131.91(8) . . ? C1 Ru C13 114.95(9) . . ? C3 Ru C13 160.45(8) . . ? C11 Ru C13 62.15(7) . . ? C12 Ru C13 37.22(7) . . ? C15 Ru C13 62.13(7) . . ? C2 Ru C14 159.46(9) . . ? C1 Ru C14 149.23(8) . . ? C3 Ru C14 142.63(8) . . ? C11 Ru C14 61.48(8) . . ? C12 Ru C14 61.60(8) . . ? C15 Ru C14 36.84(7) . . ? C13 Ru C14 36.82(7) . . ? C2 Ru P 109.71(7) . . ? C1 Ru P 87.26(7) . . ? C3 Ru P 93.55(6) . . ? C11 Ru P 148.10(7) . . ? C12 Ru P 142.70(6) . . ? C15 Ru P 110.99(7) . . ? C13 Ru P 105.77(6) . . ? C14 Ru P 90.79(6) . . ? C22 P C23 97.96(10) . . ? C22 P C21 96.37(10) . . ? C23 P C21 102.49(10) . . ? C22 P Ru 125.92(8) . . ? C23 P Ru 115.98(7) . . ? C21 P Ru 114.11(7) . . ? C2 C1 Ru 68.32(13) . . ? C1 C2 C3 118.9(2) . . ? C1 C2 C10 120.3(2) . . ? C3 C2 C10 120.77(18) . . ? C1 C2 Ru 73.20(14) . . ? C3 C2 Ru 73.89(13) . . ? C10 C2 Ru 122.85(16) . . ? C2 C3 C4 124.6(2) . . ? C2 C3 Ru 67.43(12) . . ? C4 C3 Ru 127.07(15) . . ? C9 C4 C5 116.9(2) . . ? C9 C4 C3 120.9(2) . . ? C5 C4 C3 122.1(2) . . ? C6 C5 C4 121.7(2) . . ? C7 C6 C5 120.1(2) . . ? C8 C7 C6 119.5(2) . . ? C7 C8 C9 120.4(2) . . ? C8 C9 C4 121.3(2) . . ? C15 C11 C12 108.35(19) . . ? C15 C11 C16 123.5(2) . . ? C12 C11 C16 127.4(2) . . ? C15 C11 Ru 71.78(13) . . ? C12 C11 Ru 71.53(13) . . ? C16 C11 Ru 130.27(16) . . ? C11 C12 C13 107.9(2) . . ? C11 C12 C17 128.24(19) . . ? C13 C12 C17 123.42(19) . . ? C11 C12 Ru 71.10(13) . . ? C13 C12 Ru 72.12(12) . . ? C17 C12 Ru 128.47(17) . . ? C14 C13 C12 107.40(19) . . ? C14 C13 C18 126.6(2) . . ? C12 C13 C18 125.3(2) . . ? C14 C13 Ru 72.09(12) . . ? C12 C13 Ru 70.66(13) . . ? C18 C13 Ru 130.13(15) . . ? C15 C14 C13 108.8(2) . . ? C15 C14 C19 125.0(2) . . ? C13 C14 C19 124.89(19) . . ? C15 C14 Ru 70.50(15) . . ? C13 C14 Ru 71.09(13) . . ? C19 C14 Ru 134.91(16) . . ? C14 C15 C11 107.59(19) . . ? C14 C15 C20 127.0(2) . . ? C11 C15 C20 125.0(2) . . ? C14 C15 Ru 72.67(14) . . ? C11 C15 Ru 71.03(14) . . ? C20 C15 Ru 127.58(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Ru P C22 -7.34(11) . . . . ? C1 Ru P C22 24.47(11) . . . . ? C3 Ru P C22 -43.38(11) . . . . ? C11 Ru P C22 -158.06(13) . . . . ? C12 Ru P C22 133.82(13) . . . . ? C15 Ru P C22 -154.68(10) . . . . ? C13 Ru P C22 139.64(11) . . . . ? C14 Ru P C22 173.75(10) . . . . ? C2 Ru P C23 115.56(10) . . . . ? C1 Ru P C23 147.38(10) . . . . ? C3 Ru P C23 79.52(10) . . . . ? C11 Ru P C23 -35.15(14) . . . . ? C12 Ru P C23 -103.28(13) . . . . ? C15 Ru P C23 -31.78(10) . . . . ? C13 Ru P C23 -97.46(10) . . . . ? C14 Ru P C23 -63.34(10) . . . . ? C2 Ru P C21 -125.65(10) . . . . ? C1 Ru P C21 -93.84(10) . . . . ? C3 Ru P C21 -161.69(10) . . . . ? C11 Ru P C21 83.63(14) . . . . ? C12 Ru P C21 15.51(13) . . . . ? C15 Ru P C21 87.01(10) . . . . ? C13 Ru P C21 21.33(10) . . . . ? C14 Ru P C21 55.44(10) . . . . ? C3 Ru C1 C2 -32.15(14) . . . . ? C11 Ru C1 C2 54.54(17) . . . . ? C12 Ru C1 C2 88.98(15) . . . . ? C15 Ru C1 C2 50.4(3) . . . . ? C13 Ru C1 C2 126.78(14) . . . . ? C14 Ru C1 C2 145.97(17) . . . . ? P Ru C1 C2 -127.08(14) . . . . ? Ru C1 C2 C3 60.1(2) . . . . ? Ru C1 C2 C10 -118.7(2) . . . . ? C3 Ru C2 C1 127.8(2) . . . . ? C11 Ru C2 C1 -137.32(15) . . . . ? C12 Ru C2 C1 -99.46(15) . . . . ? C15 Ru C2 C1 -162.08(14) . . . . ? C13 Ru C2 C1 -77.37(18) . . . . ? C14 Ru C2 C1 -125.3(2) . . . . ? P Ru C2 C1 57.83(15) . . . . ? C1 Ru C2 C3 -127.8(2) . . . . ? C11 Ru C2 C3 94.86(13) . . . . ? C12 Ru C2 C3 132.72(13) . . . . ? C15 Ru C2 C3 70.11(16) . . . . ? C13 Ru C2 C3 154.81(12) . . . . ? C14 Ru C2 C3 106.9(2) . . . . ? P Ru C2 C3 -69.98(13) . . . . ? C1 Ru C2 C10 115.6(2) . . . . ? C3 Ru C2 C10 -116.6(2) . . . . ? C11 Ru C2 C10 -21.71(18) . . . . ? C12 Ru C2 C10 16.15(18) . . . . ? C15 Ru C2 C10 -46.5(2) . . . . ? C13 Ru C2 C10 38.2(2) . . . . ? C14 Ru C2 C10 -9.7(3) . . . . ? P Ru C2 C10 173.44(14) . . . . ? C1 C2 C3 C4 60.6(3) . . . . ? C10 C2 C3 C4 -120.6(2) . . . . ? Ru C2 C3 C4 120.4(2) . . . . ? C1 C2 C3 Ru -59.8(2) . . . . ? C10 C2 C3 Ru 119.0(2) . . . . ? C1 Ru C3 C2 31.98(14) . . . . ? C11 Ru C3 C2 -91.55(14) . . . . ? C12 Ru C3 C2 -60.37(16) . . . . ? C15 Ru C3 C2 -128.88(14) . . . . ? C13 Ru C3 C2 -71.1(3) . . . . ? C14 Ru C3 C2 -146.42(15) . . . . ? P Ru C3 C2 117.60(12) . . . . ? C2 Ru C3 C4 -117.2(3) . . . . ? C1 Ru C3 C4 -85.2(2) . . . . ? C11 Ru C3 C4 151.3(2) . . . . ? C12 Ru C3 C4 -177.56(18) . . . . ? C15 Ru C3 C4 113.9(2) . . . . ? C13 Ru C3 C4 171.7(2) . . . . ? C14 Ru C3 C4 96.4(2) . . . . ? P Ru C3 C4 0.4(2) . . . . ? C2 C3 C4 C9 -172.3(2) . . . . ? Ru C3 C4 C9 -86.0(2) . . . . ? C2 C3 C4 C5 12.0(3) . . . . ? Ru C3 C4 C5 98.4(2) . . . . ? C9 C4 C5 C6 3.9(3) . . . . ? C3 C4 C5 C6 179.75(19) . . . . ? C4 C5 C6 C7 -1.8(3) . . . . ? C5 C6 C7 C8 -1.1(3) . . . . ? C6 C7 C8 C9 1.7(4) . . . . ? C7 C8 C9 C4 0.5(3) . . . . ? C5 C4 C9 C8 -3.3(3) . . . . ? C3 C4 C9 C8 -179.16(19) . . . . ? C2 Ru C11 C15 -147.03(13) . . . . ? C1 Ru C11 C15 -177.85(12) . . . . ? C3 Ru C11 C15 -107.86(13) . . . . ? C12 Ru C11 C15 117.35(19) . . . . ? C13 Ru C11 C15 79.73(14) . . . . ? C14 Ru C11 C15 37.74(12) . . . . ? P Ru C11 C15 5.21(19) . . . . ? C2 Ru C11 C12 95.62(14) . . . . ? C1 Ru C11 C12 64.80(16) . . . . ? C3 Ru C11 C12 134.79(14) . . . . ? C15 Ru C11 C12 -117.35(19) . . . . ? C13 Ru C11 C12 -37.62(13) . . . . ? C14 Ru C11 C12 -79.61(14) . . . . ? P Ru C11 C12 -112.13(14) . . . . ? C2 Ru C11 C16 -28.1(2) . . . . ? C1 Ru C11 C16 -59.0(2) . . . . ? C3 Ru C11 C16 11.0(2) . . . . ? C12 Ru C11 C16 -123.8(3) . . . . ? C15 Ru C11 C16 118.9(3) . . . . ? C13 Ru C11 C16 -161.4(3) . . . . ? C14 Ru C11 C16 156.6(3) . . . . ? P Ru C11 C16 124.1(2) . . . . ? C15 C11 C12 C13 0.4(3) . . . . ? C16 C11 C12 C13 -169.8(2) . . . . ? Ru C11 C12 C13 63.17(16) . . . . ? C15 C11 C12 C17 172.7(2) . . . . ? C16 C11 C12 C17 2.5(4) . . . . ? Ru C11 C12 C17 -124.6(3) . . . . ? C15 C11 C12 Ru -62.73(16) . . . . ? C16 C11 C12 Ru 127.0(2) . . . . ? C2 Ru C12 C11 -90.73(14) . . . . ? C1 Ru C12 C11 -129.92(14) . . . . ? C3 Ru C12 C11 -57.24(17) . . . . ? C15 Ru C12 C11 37.32(13) . . . . ? C13 Ru C12 C11 116.8(2) . . . . ? C14 Ru C12 C11 79.26(14) . . . . ? P Ru C12 C11 126.12(12) . . . . ? C2 Ru C12 C13 152.44(13) . . . . ? C1 Ru C12 C13 113.25(14) . . . . ? C3 Ru C12 C13 -174.07(12) . . . . ? C11 Ru C12 C13 -116.8(2) . . . . ? C15 Ru C12 C13 -79.51(14) . . . . ? C14 Ru C12 C13 -37.57(12) . . . . ? P Ru C12 C13 9.29(19) . . . . ? C2 Ru C12 C17 33.57(19) . . . . ? C1 Ru C12 C17 -5.6(2) . . . . ? C3 Ru C12 C17 67.1(2) . . . . ? C11 Ru C12 C17 124.3(2) . . . . ? C15 Ru C12 C17 161.6(2) . . . . ? C13 Ru C12 C17 -118.9(2) . . . . ? C14 Ru C12 C17 -156.4(2) . . . . ? P Ru C12 C17 -109.58(18) . . . . ? C11 C12 C13 C14 0.7(3) . . . . ? C17 C12 C13 C14 -172.1(2) . . . . ? Ru C12 C13 C14 63.16(16) . . . . ? C11 C12 C13 C18 171.5(2) . . . . ? C17 C12 C13 C18 -1.3(4) . . . . ? Ru C12 C13 C18 -126.0(2) . . . . ? C11 C12 C13 Ru -62.50(17) . . . . ? C17 C12 C13 Ru 124.8(2) . . . . ? C2 Ru C13 C14 -154.25(13) . . . . ? C1 Ru C13 C14 163.71(13) . . . . ? C3 Ru C13 C14 -101.6(3) . . . . ? C11 Ru C13 C14 -78.73(14) . . . . ? C12 Ru C13 C14 -116.51(19) . . . . ? C15 Ru C13 C14 -36.45(13) . . . . ? P Ru C13 C14 69.32(13) . . . . ? C2 Ru C13 C12 -37.74(17) . . . . ? C1 Ru C13 C12 -79.77(15) . . . . ? C3 Ru C13 C12 14.9(3) . . . . ? C11 Ru C13 C12 37.78(13) . . . . ? C15 Ru C13 C12 80.06(14) . . . . ? C14 Ru C13 C12 116.51(19) . . . . ? P Ru C13 C12 -174.17(12) . . . . ? C2 Ru C13 C18 82.6(2) . . . . ? C1 Ru C13 C18 40.6(2) . . . . ? C3 Ru C13 C18 135.3(2) . . . . ? C11 Ru C13 C18 158.2(2) . . . . ? C12 Ru C13 C18 120.4(3) . . . . ? C15 Ru C13 C18 -159.6(2) . . . . ? C14 Ru C13 C18 -123.1(3) . . . . ? P Ru C13 C18 -53.8(2) . . . . ? C12 C13 C14 C15 -1.5(3) . . . . ? C18 C13 C14 C15 -172.2(2) . . . . ? Ru C13 C14 C15 60.72(18) . . . . ? C12 C13 C14 C19 165.6(2) . . . . ? C18 C13 C14 C19 -5.0(4) . . . . ? Ru C13 C14 C19 -132.1(2) . . . . ? C12 C13 C14 Ru -62.22(16) . . . . ? C18 C13 C14 Ru 127.1(2) . . . . ? C2 Ru C14 C15 -51.7(3) . . . . ? C1 Ru C14 C15 -148.63(18) . . . . ? C3 Ru C14 C15 28.5(2) . . . . ? C11 Ru C14 C15 -38.10(13) . . . . ? C12 Ru C14 C15 -80.85(15) . . . . ? C13 Ru C14 C15 -118.8(2) . . . . ? P Ru C14 C15 125.39(13) . . . . ? C2 Ru C14 C13 67.2(3) . . . . ? C1 Ru C14 C13 -29.8(2) . . . . ? C3 Ru C14 C13 147.31(14) . . . . ? C11 Ru C14 C13 80.72(14) . . . . ? C12 Ru C14 C13 37.97(12) . . . . ? C15 Ru C14 C13 118.8(2) . . . . ? P Ru C14 C13 -115.79(12) . . . . ? C2 Ru C14 C19 -172.0(2) . . . . ? C1 Ru C14 C19 91.0(3) . . . . ? C3 Ru C14 C19 -91.9(2) . . . . ? C11 Ru C14 C19 -158.5(2) . . . . ? C12 Ru C14 C19 158.8(2) . . . . ? C15 Ru C14 C19 -120.4(3) . . . . ? C13 Ru C14 C19 120.8(3) . . . . ? P Ru C14 C19 5.0(2) . . . . ? C13 C14 C15 C11 1.8(3) . . . . ? C19 C14 C15 C11 -165.4(2) . . . . ? Ru C14 C15 C11 62.86(17) . . . . ? C13 C14 C15 C20 174.5(2) . . . . ? C19 C14 C15 C20 7.4(4) . . . . ? Ru C14 C15 C20 -124.4(2) . . . . ? C13 C14 C15 Ru -61.09(17) . . . . ? C19 C14 C15 Ru 131.8(2) . . . . ? C12 C11 C15 C14 -1.4(3) . . . . ? C16 C11 C15 C14 169.3(2) . . . . ? Ru C11 C15 C14 -63.93(17) . . . . ? C12 C11 C15 C20 -174.3(2) . . . . ? C16 C11 C15 C20 -3.6(4) . . . . ? Ru C11 C15 C20 123.1(2) . . . . ? C12 C11 C15 Ru 62.57(17) . . . . ? C16 C11 C15 Ru -126.7(2) . . . . ? C2 Ru C15 C14 159.49(14) . . . . ? C1 Ru C15 C14 121.9(3) . . . . ? C3 Ru C15 C14 -162.23(13) . . . . ? C11 Ru C15 C14 116.23(18) . . . . ? C12 Ru C15 C14 78.72(14) . . . . ? C13 Ru C15 C14 36.44(13) . . . . ? P Ru C15 C14 -60.82(14) . . . . ? C2 Ru C15 C11 43.26(16) . . . . ? C1 Ru C15 C11 5.6(3) . . . . ? C3 Ru C15 C11 81.53(14) . . . . ? C12 Ru C15 C11 -37.51(12) . . . . ? C13 Ru C15 C11 -79.79(13) . . . . ? C14 Ru C15 C11 -116.23(18) . . . . ? P Ru C15 C11 -177.05(11) . . . . ? C2 Ru C15 C20 -76.8(2) . . . . ? C1 Ru C15 C20 -114.5(3) . . . . ? C3 Ru C15 C20 -38.6(2) . . . . ? C11 Ru C15 C20 -120.1(3) . . . . ? C12 Ru C15 C20 -157.6(3) . . . . ? C13 Ru C15 C20 160.1(2) . . . . ? C14 Ru C15 C20 123.7(3) . . . . ? P Ru C15 C20 62.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.472 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.065 #============================================================================= # end of cif data for "andyg31b" (compound 2-anti) #============================================================================= #============================================================================= # cif data for "andyg59" (compound 2-syn) #============================================================================= data_andyg59 _database_code_depnum_ccdc_archive 'CCDC 832073' #TrackingRef '- andyg- chem sci.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H35 P Ru' _chemical_formula_weight 443.55 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' 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 'P 21/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 8.3388(2) _cell_length_b 17.1916(6) _cell_length_c 15.4241(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.443(4) _cell_angle_gamma 90.00 _cell_volume 2131.33(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 31906 _cell_measurement_theta_min 2.3646 _cell_measurement_theta_max 29.1742 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.814 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94618 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63644 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4865 _reflns_number_gt 4456 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _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^)+(0.0165P)^2^+1.4419P] 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 ; The hydrogens of the C1 and C3 atoms were refined freely. The methyls were refined using a rigid model, others riding. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4865 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0221 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0441 _refine_ls_wR_factor_gt 0.0426 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Ru Ru 0.969522(13) 0.456265(6) 0.768142(7) 0.00939(4) Uani 1 1 d . . . P P 1.14755(5) 0.54798(2) 0.73820(3) 0.01533(8) Uani 1 1 d . . . C1 C 1.16951(19) 0.41155(9) 0.87692(10) 0.0167(3) Uani 1 1 d . . . H1A H 1.274(2) 0.4386(10) 0.8840(11) 0.017(4) Uiso 1 1 d . . . H1B H 1.147(2) 0.4011(10) 0.9340(12) 0.019(4) Uiso 1 1 d . . . C2 C 1.11575(17) 0.35426(8) 0.80789(10) 0.0143(3) Uani 1 1 d . . . C3 C 1.14107(17) 0.37510(8) 0.72221(10) 0.0138(3) Uani 1 1 d . . . H3 H 1.242(2) 0.4034(10) 0.7252(11) 0.013(4) Uiso 1 1 d . . . C4 C 1.09534(18) 0.32694(8) 0.63970(9) 0.0140(3) Uani 1 1 d . . . C5 C 1.21023(19) 0.31875(9) 0.58835(10) 0.0171(3) Uani 1 1 d . . . H5 H 1.3143 0.3448 0.6070 0.021 Uiso 1 1 calc R . . C6 C 1.1755(2) 0.27355(9) 0.51090(10) 0.0214(3) Uani 1 1 d . . . H6 H 1.2560 0.2686 0.4777 0.026 Uiso 1 1 calc R . . C7 C 1.0241(2) 0.23559(9) 0.48176(10) 0.0218(3) Uani 1 1 d . . . H7 H 1.0004 0.2044 0.4290 0.026 Uiso 1 1 calc R . . C8 C 0.9076(2) 0.24380(9) 0.53085(10) 0.0199(3) Uani 1 1 d . . . H8 H 0.8030 0.2183 0.5113 0.024 Uiso 1 1 calc R . . C9 C 0.94261(18) 0.28890(9) 0.60816(10) 0.0170(3) Uani 1 1 d . . . H9 H 0.8609 0.2941 0.6405 0.020 Uiso 1 1 calc R . . C10 C 1.04797(19) 0.27726(8) 0.82878(10) 0.0182(3) Uani 1 1 d . . . H10A H 1.1398 0.2404 0.8496 0.027 Uiso 1 1 calc R . . H10B H 0.9696 0.2569 0.7744 0.027 Uiso 1 1 calc R . . H10C H 0.9904 0.2845 0.8759 0.027 Uiso 1 1 calc R . . C11 C 0.76747(17) 0.45665(8) 0.83678(9) 0.0123(3) Uani 1 1 d . . . C12 C 0.71522(16) 0.40454(8) 0.76210(9) 0.0122(3) Uani 1 1 d . . . C13 C 0.70141(16) 0.44814(8) 0.68139(9) 0.0121(3) Uani 1 1 d . . . C14 C 0.74235(16) 0.52685(8) 0.70597(9) 0.0124(3) Uani 1 1 d . . . C15 C 0.78380(16) 0.53284(8) 0.80301(9) 0.0116(3) Uani 1 1 d . . . C16 C 0.78053(19) 0.43708(9) 0.93331(10) 0.0175(3) Uani 1 1 d . . . H16A H 0.8562 0.4738 0.9726 0.026 Uiso 1 1 calc R . . H16B H 0.8237 0.3841 0.9461 0.026 Uiso 1 1 calc R . . H16C H 0.6702 0.4406 0.9442 0.026 Uiso 1 1 calc R . . C17 C 0.65037(18) 0.32359(8) 0.76713(10) 0.0157(3) Uani 1 1 d . . . H17A H 0.5321 0.3260 0.7654 0.024 Uiso 1 1 calc R . . H17B H 0.7125 0.2990 0.8233 0.024 Uiso 1 1 calc R . . H17C H 0.6642 0.2931 0.7160 0.024 Uiso 1 1 calc R . . C18 C 0.63067(18) 0.42087(9) 0.58634(10) 0.0175(3) Uani 1 1 d . . . H18A H 0.5215 0.4449 0.5614 0.026 Uiso 1 1 calc R . . H18B H 0.6186 0.3642 0.5857 0.026 Uiso 1 1 calc R . . H18C H 0.7057 0.4357 0.5499 0.026 Uiso 1 1 calc R . . C19 C 0.70859(19) 0.59276(9) 0.63996(10) 0.0184(3) Uani 1 1 d . . . H19A H 0.7538 0.5802 0.5892 0.028 Uiso 1 1 calc R . . H19B H 0.7616 0.6402 0.6695 0.028 Uiso 1 1 calc R . . H19C H 0.5883 0.6010 0.6181 0.028 Uiso 1 1 calc R . . C20 C 0.80459(18) 0.60590(8) 0.85779(10) 0.0161(3) Uani 1 1 d . . . H20A H 0.7054 0.6143 0.8793 0.024 Uiso 1 1 calc R . . H20B H 0.8195 0.6501 0.8206 0.024 Uiso 1 1 calc R . . H20C H 0.9025 0.6011 0.9094 0.024 Uiso 1 1 calc R . . C21 C 1.1181(2) 0.65014(9) 0.76363(13) 0.0272(4) Uani 1 1 d . . . H21A H 1.2022 0.6821 0.7466 0.041 Uiso 1 1 calc R . . H21B H 1.1295 0.6560 0.8282 0.041 Uiso 1 1 calc R . . H21C H 1.0069 0.6671 0.7297 0.041 Uiso 1 1 calc R . . C22 C 1.37200(19) 0.54408(10) 0.79126(13) 0.0281(4) Uani 1 1 d . . . H22A H 1.4277 0.5854 0.7666 0.042 Uiso 1 1 calc R . . H22B H 1.4155 0.4934 0.7792 0.042 Uiso 1 1 calc R . . H22C H 1.3928 0.5513 0.8563 0.042 Uiso 1 1 calc R . . C23 C 1.1478(2) 0.55421(10) 0.61957(12) 0.0255(4) Uani 1 1 d . . . H23A H 1.0359 0.5675 0.5830 0.038 Uiso 1 1 calc R . . H23B H 1.1813 0.5040 0.5999 0.038 Uiso 1 1 calc R . . H23C H 1.2264 0.5945 0.6123 0.038 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 Ru 0.00869(6) 0.00930(6) 0.00999(6) -0.00107(4) 0.00216(4) 0.00031(4) P 0.01228(17) 0.01351(18) 0.0218(2) -0.00307(14) 0.00737(15) -0.00238(13) C1 0.0154(7) 0.0187(7) 0.0139(7) -0.0008(6) 0.0004(6) 0.0054(6) C2 0.0121(6) 0.0139(7) 0.0154(7) -0.0004(5) 0.0012(5) 0.0055(5) C3 0.0104(6) 0.0139(7) 0.0170(7) -0.0034(5) 0.0034(5) 0.0013(5) C4 0.0172(7) 0.0112(6) 0.0144(7) 0.0008(5) 0.0053(6) 0.0023(5) C5 0.0186(7) 0.0151(7) 0.0194(7) 0.0012(6) 0.0082(6) 0.0020(6) C6 0.0307(8) 0.0192(7) 0.0192(8) 0.0019(6) 0.0150(7) 0.0053(6) C7 0.0368(9) 0.0158(7) 0.0138(7) -0.0021(6) 0.0082(6) -0.0001(6) C8 0.0264(8) 0.0165(7) 0.0163(7) -0.0004(6) 0.0045(6) -0.0054(6) C9 0.0183(7) 0.0184(7) 0.0153(7) -0.0007(6) 0.0062(6) -0.0006(6) C10 0.0223(8) 0.0154(7) 0.0166(7) 0.0015(6) 0.0045(6) 0.0052(6) C11 0.0104(6) 0.0136(7) 0.0133(7) 0.0002(5) 0.0041(5) 0.0006(5) C12 0.0095(6) 0.0132(7) 0.0139(7) -0.0003(5) 0.0034(5) 0.0000(5) C13 0.0085(6) 0.0149(7) 0.0126(7) 0.0002(5) 0.0025(5) -0.0001(5) C14 0.0090(6) 0.0148(7) 0.0131(7) 0.0009(5) 0.0024(5) 0.0010(5) C15 0.0083(6) 0.0128(6) 0.0138(7) -0.0003(5) 0.0031(5) 0.0014(5) C16 0.0217(7) 0.0187(7) 0.0133(7) 0.0008(6) 0.0068(6) -0.0014(6) C17 0.0167(7) 0.0139(7) 0.0172(7) 0.0006(5) 0.0058(6) -0.0033(5) C18 0.0179(7) 0.0198(7) 0.0132(7) -0.0001(6) 0.0015(6) -0.0031(6) C19 0.0189(7) 0.0168(7) 0.0178(7) 0.0035(6) 0.0015(6) 0.0001(6) C20 0.0164(7) 0.0136(7) 0.0183(7) -0.0024(6) 0.0049(6) 0.0009(5) C21 0.0284(9) 0.0138(7) 0.0452(11) -0.0064(7) 0.0195(8) -0.0067(6) C22 0.0137(7) 0.0292(9) 0.0411(10) -0.0050(8) 0.0070(7) -0.0062(6) C23 0.0302(9) 0.0231(8) 0.0280(9) 0.0004(7) 0.0164(7) -0.0053(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C2 2.1308(13) . ? Ru C1 2.1672(14) . ? Ru C15 2.2055(13) . ? Ru C11 2.2158(13) . ? Ru C14 2.2390(13) . ? Ru C3 2.2439(13) . ? Ru C12 2.2784(13) . ? Ru C13 2.2837(14) . ? Ru P 2.2953(4) . ? P C21 1.8303(16) . ? P C22 1.8335(17) . ? P C23 1.8335(17) . ? C1 C2 1.432(2) . ? C2 C3 1.438(2) . ? C2 C10 1.507(2) . ? C3 C4 1.4805(19) . ? C4 C9 1.399(2) . ? C4 C5 1.4033(19) . ? C5 C6 1.390(2) . ? C6 C7 1.385(2) . ? C7 C8 1.389(2) . ? C8 C9 1.387(2) . ? C11 C15 1.4294(19) . ? C11 C12 1.4326(19) . ? C11 C16 1.5018(19) . ? C12 C13 1.4312(19) . ? C12 C17 1.5024(19) . ? C13 C14 1.4221(19) . ? C13 C18 1.5021(19) . ? C14 C15 1.4474(19) . ? C14 C19 1.4990(19) . ? C15 C20 1.4979(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Ru C1 38.91(5) . . ? C2 Ru C15 143.74(5) . . ? C1 Ru C15 117.93(5) . . ? C2 Ru C11 108.34(5) . . ? C1 Ru C11 99.06(5) . . ? C15 Ru C11 37.72(5) . . ? C2 Ru C14 157.43(5) . . ? C1 Ru C14 155.88(5) . . ? C15 Ru C14 38.00(5) . . ? C11 Ru C14 62.53(5) . . ? C2 Ru C3 38.28(5) . . ? C1 Ru C3 66.43(5) . . ? C15 Ru C3 175.04(5) . . ? C11 Ru C3 141.50(5) . . ? C14 Ru C3 137.70(5) . . ? C2 Ru C12 98.37(5) . . ? C1 Ru C12 114.15(6) . . ? C15 Ru C12 62.40(5) . . ? C11 Ru C12 37.14(5) . . ? C14 Ru C12 61.44(5) . . ? C3 Ru C12 114.14(5) . . ? C2 Ru C13 120.95(5) . . ? C1 Ru C13 149.70(6) . . ? C15 Ru C13 62.48(5) . . ? C11 Ru C13 61.95(5) . . ? C14 Ru C13 36.64(5) . . ? C3 Ru C13 112.58(5) . . ? C12 Ru C13 36.57(5) . . ? C2 Ru P 105.79(4) . . ? C1 Ru P 89.65(4) . . ? C15 Ru P 99.95(4) . . ? C11 Ru P 135.14(4) . . ? C14 Ru P 93.46(4) . . ? C3 Ru P 82.11(4) . . ? C12 Ru P 154.78(4) . . ? C13 Ru P 120.59(4) . . ? C21 P C22 96.82(8) . . ? C21 P C23 101.17(8) . . ? C22 P C23 100.09(8) . . ? C21 P Ru 119.03(5) . . ? C22 P Ru 121.54(6) . . ? C23 P Ru 114.43(6) . . ? C2 C1 Ru 69.17(8) . . ? C1 C2 C3 114.73(13) . . ? C1 C2 C10 120.40(13) . . ? C3 C2 C10 124.78(13) . . ? C1 C2 Ru 71.92(8) . . ? C3 C2 Ru 75.12(8) . . ? C10 C2 Ru 124.45(10) . . ? C2 C3 C4 125.68(13) . . ? C2 C3 Ru 66.60(7) . . ? C4 C3 Ru 125.39(10) . . ? C9 C4 C5 116.87(13) . . ? C9 C4 C3 124.25(13) . . ? C5 C4 C3 118.88(13) . . ? C6 C5 C4 121.60(14) . . ? C7 C6 C5 120.39(14) . . ? C6 C7 C8 118.98(14) . . ? C9 C8 C7 120.52(14) . . ? C8 C9 C4 121.62(14) . . ? C15 C11 C12 108.55(12) . . ? C15 C11 C16 125.30(12) . . ? C12 C11 C16 125.68(12) . . ? C15 C11 Ru 70.75(8) . . ? C12 C11 Ru 73.80(8) . . ? C16 C11 Ru 127.54(10) . . ? C13 C12 C11 107.98(12) . . ? C13 C12 C17 125.69(12) . . ? C11 C12 C17 125.05(12) . . ? C13 C12 Ru 71.92(8) . . ? C11 C12 Ru 69.06(7) . . ? C17 C12 Ru 134.69(10) . . ? C14 C13 C12 107.97(12) . . ? C14 C13 C18 124.14(13) . . ? C12 C13 C18 127.24(13) . . ? C14 C13 Ru 69.97(8) . . ? C12 C13 Ru 71.51(8) . . ? C18 C13 Ru 131.27(10) . . ? C13 C14 C15 108.52(12) . . ? C13 C14 C19 123.36(13) . . ? C15 C14 C19 126.76(13) . . ? C13 C14 Ru 73.39(8) . . ? C15 C14 Ru 69.75(7) . . ? C19 C14 Ru 133.24(10) . . ? C11 C15 C14 106.98(12) . . ? C11 C15 C20 124.80(12) . . ? C14 C15 C20 127.08(12) . . ? C11 C15 Ru 71.53(8) . . ? C14 C15 Ru 72.25(7) . . ? C20 C15 Ru 130.90(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Ru P C21 -145.72(8) . . . . ? C1 Ru P C21 -109.85(8) . . . . ? C15 Ru P C21 8.48(8) . . . . ? C11 Ru P C21 -7.32(9) . . . . ? C14 Ru P C21 46.21(8) . . . . ? C3 Ru P C21 -176.09(8) . . . . ? C12 Ru P C21 51.46(11) . . . . ? C13 Ru P C21 72.29(8) . . . . ? C2 Ru P C22 -25.72(8) . . . . ? C1 Ru P C22 10.15(8) . . . . ? C15 Ru P C22 128.48(8) . . . . ? C11 Ru P C22 112.68(9) . . . . ? C14 Ru P C22 166.21(8) . . . . ? C3 Ru P C22 -56.09(8) . . . . ? C12 Ru P C22 171.45(11) . . . . ? C13 Ru P C22 -167.71(8) . . . . ? C2 Ru P C23 94.59(7) . . . . ? C1 Ru P C23 130.45(7) . . . . ? C15 Ru P C23 -111.22(7) . . . . ? C11 Ru P C23 -127.01(8) . . . . ? C14 Ru P C23 -73.49(7) . . . . ? C3 Ru P C23 64.22(7) . . . . ? C12 Ru P C23 -68.24(11) . . . . ? C13 Ru P C23 -47.40(8) . . . . ? C15 Ru C1 C2 142.76(8) . . . . ? C11 Ru C1 C2 108.05(9) . . . . ? C14 Ru C1 C2 146.16(12) . . . . ? C3 Ru C1 C2 -34.61(8) . . . . ? C12 Ru C1 C2 72.46(9) . . . . ? C13 Ru C1 C2 60.19(14) . . . . ? P Ru C1 C2 -116.15(8) . . . . ? Ru C1 C2 C3 63.40(11) . . . . ? Ru C1 C2 C10 -119.90(13) . . . . ? C15 Ru C2 C1 -64.67(12) . . . . ? C11 Ru C2 C1 -81.57(9) . . . . ? C14 Ru C2 C1 -143.64(13) . . . . ? C3 Ru C2 C1 122.82(12) . . . . ? C12 Ru C2 C1 -118.43(9) . . . . ? C13 Ru C2 C1 -149.31(8) . . . . ? P Ru C2 C1 68.87(9) . . . . ? C1 Ru C2 C3 -122.82(12) . . . . ? C15 Ru C2 C3 172.50(8) . . . . ? C11 Ru C2 C3 155.61(8) . . . . ? C14 Ru C2 C3 93.54(15) . . . . ? C12 Ru C2 C3 118.74(8) . . . . ? C13 Ru C2 C3 87.87(9) . . . . ? P Ru C2 C3 -53.95(8) . . . . ? C1 Ru C2 C10 114.93(15) . . . . ? C15 Ru C2 C10 50.26(16) . . . . ? C11 Ru C2 C10 33.37(13) . . . . ? C14 Ru C2 C10 -28.7(2) . . . . ? C3 Ru C2 C10 -122.24(16) . . . . ? C12 Ru C2 C10 -3.50(12) . . . . ? C13 Ru C2 C10 -34.37(14) . . . . ? P Ru C2 C10 -176.19(11) . . . . ? C1 C2 C3 C4 -179.37(13) . . . . ? C10 C2 C3 C4 4.1(2) . . . . ? Ru C2 C3 C4 -117.79(13) . . . . ? C1 C2 C3 Ru -61.58(10) . . . . ? C10 C2 C3 Ru 121.89(14) . . . . ? C1 Ru C3 C2 35.16(8) . . . . ? C15 Ru C3 C2 -116.9(6) . . . . ? C11 Ru C3 C2 -39.02(12) . . . . ? C14 Ru C3 C2 -145.31(9) . . . . ? C12 Ru C3 C2 -71.91(9) . . . . ? C13 Ru C3 C2 -111.84(8) . . . . ? P Ru C3 C2 128.24(8) . . . . ? C2 Ru C3 C4 118.18(15) . . . . ? C1 Ru C3 C4 153.34(14) . . . . ? C15 Ru C3 C4 1.3(7) . . . . ? C11 Ru C3 C4 79.16(15) . . . . ? C14 Ru C3 C4 -27.13(16) . . . . ? C12 Ru C3 C4 46.26(13) . . . . ? C13 Ru C3 C4 6.33(14) . . . . ? P Ru C3 C4 -113.59(12) . . . . ? C2 C3 C4 C9 45.8(2) . . . . ? Ru C3 C4 C9 -39.0(2) . . . . ? C2 C3 C4 C5 -134.82(15) . . . . ? Ru C3 C4 C5 140.32(12) . . . . ? C9 C4 C5 C6 -1.4(2) . . . . ? C3 C4 C5 C6 179.16(14) . . . . ? C4 C5 C6 C7 0.6(2) . . . . ? C5 C6 C7 C8 0.4(2) . . . . ? C6 C7 C8 C9 -0.4(2) . . . . ? C7 C8 C9 C4 -0.5(2) . . . . ? C5 C4 C9 C8 1.4(2) . . . . ? C3 C4 C9 C8 -179.26(14) . . . . ? C2 Ru C11 C15 163.69(8) . . . . ? C1 Ru C11 C15 124.70(8) . . . . ? C14 Ru C11 C15 -38.79(8) . . . . ? C3 Ru C11 C15 -172.06(8) . . . . ? C12 Ru C11 C15 -116.90(11) . . . . ? C13 Ru C11 C15 -80.39(8) . . . . ? P Ru C11 C15 25.99(10) . . . . ? C2 Ru C11 C12 -79.42(9) . . . . ? C1 Ru C11 C12 -118.41(8) . . . . ? C15 Ru C11 C12 116.90(11) . . . . ? C14 Ru C11 C12 78.11(8) . . . . ? C3 Ru C11 C12 -55.16(12) . . . . ? C13 Ru C11 C12 36.51(8) . . . . ? P Ru C11 C12 142.89(7) . . . . ? C2 Ru C11 C16 43.45(13) . . . . ? C1 Ru C11 C16 4.46(13) . . . . ? C15 Ru C11 C16 -120.23(16) . . . . ? C14 Ru C11 C16 -159.02(14) . . . . ? C3 Ru C11 C16 67.71(15) . . . . ? C12 Ru C11 C16 122.87(16) . . . . ? C13 Ru C11 C16 159.38(14) . . . . ? P Ru C11 C16 -94.24(12) . . . . ? C15 C11 C12 C13 0.90(15) . . . . ? C16 C11 C12 C13 173.33(13) . . . . ? Ru C11 C12 C13 -61.73(9) . . . . ? C15 C11 C12 C17 -166.72(13) . . . . ? C16 C11 C12 C17 5.7(2) . . . . ? Ru C11 C12 C17 130.65(13) . . . . ? C15 C11 C12 Ru 62.63(9) . . . . ? C16 C11 C12 Ru -124.93(14) . . . . ? C2 Ru C12 C13 -132.38(8) . . . . ? C1 Ru C12 C13 -169.63(8) . . . . ? C15 Ru C12 C13 80.19(8) . . . . ? C11 Ru C12 C13 118.20(11) . . . . ? C14 Ru C12 C13 36.90(8) . . . . ? C3 Ru C12 C13 -95.85(9) . . . . ? P Ru C12 C13 30.93(13) . . . . ? C2 Ru C12 C11 109.42(8) . . . . ? C1 Ru C12 C11 72.17(9) . . . . ? C15 Ru C12 C11 -38.01(8) . . . . ? C14 Ru C12 C11 -81.30(9) . . . . ? C3 Ru C12 C11 145.95(8) . . . . ? C13 Ru C12 C11 -118.20(11) . . . . ? P Ru C12 C11 -87.27(11) . . . . ? C2 Ru C12 C17 -9.68(14) . . . . ? C1 Ru C12 C17 -46.93(15) . . . . ? C15 Ru C12 C17 -157.11(15) . . . . ? C11 Ru C12 C17 -119.10(17) . . . . ? C14 Ru C12 C17 159.59(15) . . . . ? C3 Ru C12 C17 26.85(15) . . . . ? C13 Ru C12 C17 122.70(17) . . . . ? P Ru C12 C17 153.63(10) . . . . ? C11 C12 C13 C14 -0.87(15) . . . . ? C17 C12 C13 C14 166.65(13) . . . . ? Ru C12 C13 C14 -60.79(9) . . . . ? C11 C12 C13 C18 -171.80(13) . . . . ? C17 C12 C13 C18 -4.3(2) . . . . ? Ru C12 C13 C18 128.28(14) . . . . ? C11 C12 C13 Ru 59.92(9) . . . . ? C17 C12 C13 Ru -132.56(13) . . . . ? C2 Ru C13 C14 176.36(8) . . . . ? C1 Ru C13 C14 136.90(11) . . . . ? C15 Ru C13 C14 37.97(8) . . . . ? C11 Ru C13 C14 80.83(8) . . . . ? C3 Ru C13 C14 -141.55(8) . . . . ? C12 Ru C13 C14 117.91(11) . . . . ? P Ru C13 C14 -47.35(9) . . . . ? C2 Ru C13 C12 58.45(9) . . . . ? C1 Ru C13 C12 18.99(14) . . . . ? C15 Ru C13 C12 -79.95(8) . . . . ? C11 Ru C13 C12 -37.08(8) . . . . ? C14 Ru C13 C12 -117.91(11) . . . . ? C3 Ru C13 C12 100.54(8) . . . . ? P Ru C13 C12 -165.26(7) . . . . ? C2 Ru C13 C18 -65.30(14) . . . . ? C1 Ru C13 C18 -104.75(15) . . . . ? C15 Ru C13 C18 156.31(14) . . . . ? C11 Ru C13 C18 -160.82(15) . . . . ? C14 Ru C13 C18 118.35(16) . . . . ? C3 Ru C13 C18 -23.20(14) . . . . ? C12 Ru C13 C18 -123.74(16) . . . . ? P Ru C13 C18 71.00(13) . . . . ? C12 C13 C14 C15 0.51(15) . . . . ? C18 C13 C14 C15 171.79(12) . . . . ? Ru C13 C14 C15 -61.26(9) . . . . ? C12 C13 C14 C19 -166.97(13) . . . . ? C18 C13 C14 C19 4.3(2) . . . . ? Ru C13 C14 C19 131.26(13) . . . . ? C12 C13 C14 Ru 61.77(9) . . . . ? C18 C13 C14 Ru -126.95(13) . . . . ? C2 Ru C14 C13 -8.16(17) . . . . ? C1 Ru C14 C13 -122.49(14) . . . . ? C15 Ru C14 C13 -117.61(11) . . . . ? C11 Ru C14 C13 -79.10(8) . . . . ? C3 Ru C14 C13 58.56(11) . . . . ? C12 Ru C14 C13 -36.83(8) . . . . ? P Ru C14 C13 140.63(7) . . . . ? C2 Ru C14 C15 109.44(14) . . . . ? C1 Ru C14 C15 -4.89(17) . . . . ? C11 Ru C14 C15 38.50(8) . . . . ? C3 Ru C14 C15 176.16(8) . . . . ? C12 Ru C14 C15 80.78(8) . . . . ? C13 Ru C14 C15 117.61(11) . . . . ? P Ru C14 C15 -101.76(7) . . . . ? C2 Ru C14 C19 -128.64(15) . . . . ? C1 Ru C14 C19 117.03(16) . . . . ? C15 Ru C14 C19 121.92(17) . . . . ? C11 Ru C14 C19 160.42(15) . . . . ? C3 Ru C14 C19 -61.92(16) . . . . ? C12 Ru C14 C19 -157.30(15) . . . . ? C13 Ru C14 C19 -120.47(17) . . . . ? P Ru C14 C19 20.16(14) . . . . ? C12 C11 C15 C14 -0.58(15) . . . . ? C16 C11 C15 C14 -173.05(13) . . . . ? Ru C11 C15 C14 64.02(9) . . . . ? C12 C11 C15 C20 167.92(12) . . . . ? C16 C11 C15 C20 -4.6(2) . . . . ? Ru C11 C15 C20 -127.48(13) . . . . ? C12 C11 C15 Ru -64.60(9) . . . . ? C16 C11 C15 Ru 122.93(14) . . . . ? C13 C14 C15 C11 0.04(15) . . . . ? C19 C14 C15 C11 166.98(13) . . . . ? Ru C14 C15 C11 -63.54(9) . . . . ? C13 C14 C15 C20 -168.11(13) . . . . ? C19 C14 C15 C20 -1.2(2) . . . . ? Ru C14 C15 C20 128.31(14) . . . . ? C13 C14 C15 Ru 63.58(9) . . . . ? C19 C14 C15 Ru -129.48(14) . . . . ? C2 Ru C15 C11 -26.79(13) . . . . ? C1 Ru C15 C11 -66.78(10) . . . . ? C14 Ru C15 C11 115.48(11) . . . . ? C3 Ru C15 C11 84.1(6) . . . . ? C12 Ru C15 C11 37.42(8) . . . . ? C13 Ru C15 C11 78.87(8) . . . . ? P Ru C15 C11 -161.71(7) . . . . ? C2 Ru C15 C14 -142.27(9) . . . . ? C1 Ru C15 C14 177.74(8) . . . . ? C11 Ru C15 C14 -115.48(11) . . . . ? C3 Ru C15 C14 -31.4(6) . . . . ? C12 Ru C15 C14 -78.05(8) . . . . ? C13 Ru C15 C14 -36.60(8) . . . . ? P Ru C15 C14 82.81(7) . . . . ? C2 Ru C15 C20 93.65(15) . . . . ? C1 Ru C15 C20 53.66(14) . . . . ? C11 Ru C15 C20 120.45(16) . . . . ? C14 Ru C15 C20 -124.08(16) . . . . ? C3 Ru C15 C20 -155.5(5) . . . . ? C12 Ru C15 C20 157.87(15) . . . . ? C13 Ru C15 C20 -160.68(14) . . . . ? P Ru C15 C20 -41.26(13) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.360 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.054 #============================================================================= # end of cif data for "andyg59" (compound 2-syn) #============================================================================= #============================================================================= # cif data for "andyg35a" (compound 3) #============================================================================= data_andyg35a _database_code_depnum_ccdc_archive 'CCDC 832074' #TrackingRef '- andyg- chem sci.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H26 O Ru' _chemical_formula_weight 395.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 11.5667(2) _cell_length_b 12.0145(2) _cell_length_c 13.0890(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1818.95(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15625 _cell_measurement_theta_min 3.3738 _cell_measurement_theta_max 75.6875 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 6.973 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.66633 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20543 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0148 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 75.87 _reflns_number_total 3651 _reflns_number_gt 3478 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _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^)+(0.0356P)^2^+0.2598P] 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 ; The hydrogens of the C1 and C3 atoms were refined freely. The methyls were refined using a rigid model, others riding. ; _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 0.000(8) _refine_ls_number_reflns 3651 _refine_ls_number_parameters 226 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0203 _refine_ls_R_factor_gt 0.0193 _refine_ls_wR_factor_ref 0.0534 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 Ru Ru 0.396263(9) 0.502540(8) 0.44305(5) 0.01784(6) Uani 1 1 d . . . O O 0.31048(13) 0.69257(12) 0.57255(13) 0.0402(4) Uani 1 1 d . . . C1 C 0.42785(16) 0.40915(18) 0.58657(16) 0.0281(4) Uani 1 1 d . . . H1A H 0.402(2) 0.457(3) 0.643(2) 0.040(7) Uiso 1 1 d . . . H1B H 0.507(2) 0.374(2) 0.5959(17) 0.033(6) Uiso 1 1 d . . . C2 C 0.35072(16) 0.35066(15) 0.52248(15) 0.0228(4) Uani 1 1 d . . . C3 C 0.24463(15) 0.40133(14) 0.48988(15) 0.0209(3) Uani 1 1 d . . . H3 H 0.2134(17) 0.3660(17) 0.4325(18) 0.022(5) Uiso 1 1 d . . . C4 C 0.15831(14) 0.45702(14) 0.55653(14) 0.0215(4) Uani 1 1 d . . . C5 C 0.16405(17) 0.45464(17) 0.66263(16) 0.0279(4) Uani 1 1 d . . . H5 H 0.2252 0.4151 0.6947 0.033 Uiso 1 1 calc R . . C6 C 0.0824(3) 0.50878(16) 0.7231(3) 0.0327(6) Uani 1 1 d . . . H6 H 0.0899 0.5087 0.7954 0.039 Uiso 1 1 calc R . . C7 C -0.01036(16) 0.56302(16) 0.67685(17) 0.0308(4) Uani 1 1 d . . . H7 H -0.0671 0.5992 0.7174 0.037 Uiso 1 1 calc R . . C8 C -0.01908(15) 0.56371(16) 0.57174(18) 0.0319(4) Uani 1 1 d . . . H8 H -0.0825 0.6003 0.5401 0.038 Uiso 1 1 calc R . . C9 C 0.0640(2) 0.51145(15) 0.51161(19) 0.0259(4) Uani 1 1 d . . . H9 H 0.0566 0.5127 0.4393 0.031 Uiso 1 1 calc R . . C10 C 0.38618(17) 0.24025(17) 0.47824(19) 0.0329(5) Uani 1 1 d . . . H10A H 0.4704 0.2325 0.4824 0.039 Uiso 1 1 calc R . . H10B H 0.3619 0.2362 0.4066 0.039 Uiso 1 1 calc R . . H10C H 0.3494 0.1801 0.5169 0.039 Uiso 1 1 calc R . . C11 C 0.42380(18) 0.45188(18) 0.27741(15) 0.0218(4) Uani 1 1 d . . . C12 C 0.53096(16) 0.44110(15) 0.32939(15) 0.0220(3) Uani 1 1 d . . . C13 C 0.56368(15) 0.54795(16) 0.36879(15) 0.0222(4) Uani 1 1 d . . . C14 C 0.47616(15) 0.62470(15) 0.33876(15) 0.0231(3) Uani 1 1 d . . . C15 C 0.38787(15) 0.56595(19) 0.28396(17) 0.0234(4) Uani 1 1 d . . . C16 C 0.36354(18) 0.36356(18) 0.21588(15) 0.0317(4) Uani 1 1 d . . . H16A H 0.2797 0.3739 0.2209 0.038 Uiso 1 1 calc R . . H16B H 0.3844 0.2900 0.2424 0.038 Uiso 1 1 calc R . . H16C H 0.3873 0.3693 0.1442 0.038 Uiso 1 1 calc R . . C17 C 0.60664(16) 0.33940(18) 0.33350(19) 0.0312(4) Uani 1 1 d . . . H17A H 0.5608 0.2735 0.3159 0.037 Uiso 1 1 calc R . . H17B H 0.6380 0.3309 0.4026 0.037 Uiso 1 1 calc R . . H17C H 0.6703 0.3475 0.2847 0.037 Uiso 1 1 calc R . . C18 C 0.67531(16) 0.57431(18) 0.42146(15) 0.0304(4) Uani 1 1 d . . . H18A H 0.7354 0.5882 0.3703 0.037 Uiso 1 1 calc R . . H18B H 0.6981 0.5113 0.4645 0.037 Uiso 1 1 calc R . . H18C H 0.6654 0.6407 0.4641 0.037 Uiso 1 1 calc R . . C19 C 0.48149(18) 0.74813(16) 0.35265(18) 0.0330(4) Uani 1 1 d . . . H19A H 0.5283 0.7656 0.4130 0.040 Uiso 1 1 calc R . . H19B H 0.4031 0.7774 0.3620 0.040 Uiso 1 1 calc R . . H19C H 0.5166 0.7822 0.2921 0.040 Uiso 1 1 calc R . . C20 C 0.28574(17) 0.61808(19) 0.23084(17) 0.0330(4) Uani 1 1 d . . . H20A H 0.3090 0.6433 0.1626 0.040 Uiso 1 1 calc R . . H20B H 0.2582 0.6818 0.2707 0.040 Uiso 1 1 calc R . . H20C H 0.2236 0.5631 0.2246 0.040 Uiso 1 1 calc R . . C21 C 0.34178(18) 0.61651(17) 0.52563(17) 0.0290(4) 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 Ru 0.01461(8) 0.01927(8) 0.01966(9) -0.00140(6) 0.00069(8) -0.00069(4) O 0.0481(8) 0.0274(7) 0.0451(9) -0.0125(7) 0.0227(7) -0.0049(6) C1 0.0215(8) 0.0381(11) 0.0247(10) 0.0064(9) -0.0017(8) 0.0025(8) C2 0.0205(9) 0.0220(8) 0.0258(9) 0.0073(8) 0.0048(7) -0.0006(7) C3 0.0186(8) 0.0205(8) 0.0236(9) -0.0002(7) -0.0009(7) -0.0037(7) C4 0.0159(7) 0.0162(8) 0.0324(10) 0.0015(7) -0.0003(7) -0.0016(6) C5 0.0242(9) 0.0296(10) 0.0299(10) 0.0051(8) 0.0038(8) 0.0045(8) C6 0.0279(11) 0.0358(13) 0.0343(15) 0.0006(8) 0.0099(11) 0.0002(7) C7 0.0202(9) 0.0243(9) 0.0479(13) -0.0053(8) 0.0108(9) 0.0004(7) C8 0.0181(7) 0.0263(9) 0.0513(12) 0.0008(9) -0.0021(9) 0.0019(7) C9 0.0195(11) 0.0283(10) 0.0298(12) 0.0012(8) -0.0050(9) -0.0011(7) C10 0.0277(9) 0.0253(10) 0.0455(13) 0.0048(8) 0.0082(8) 0.0052(7) C11 0.0209(8) 0.0241(10) 0.0203(10) -0.0017(8) 0.0017(8) -0.0008(8) C12 0.0203(8) 0.0251(9) 0.0207(8) -0.0010(7) 0.0040(7) 0.0027(7) C13 0.0177(8) 0.0254(10) 0.0235(9) -0.0007(7) 0.0041(7) -0.0031(7) C14 0.0192(7) 0.0246(9) 0.0254(9) 0.0015(7) 0.0059(7) -0.0016(7) C15 0.0213(9) 0.0261(10) 0.0229(10) 0.0055(8) 0.0015(7) 0.0012(7) C16 0.0319(11) 0.0362(11) 0.0271(11) -0.0062(8) -0.0028(8) -0.0051(8) C17 0.0298(10) 0.0310(10) 0.0329(11) -0.0006(9) 0.0032(8) 0.0076(7) C18 0.0177(8) 0.0440(11) 0.0295(12) -0.0034(8) 0.0010(7) -0.0051(7) C19 0.0327(9) 0.0231(9) 0.0434(12) -0.0010(8) 0.0097(9) -0.0016(8) C20 0.0208(9) 0.0422(11) 0.0358(11) 0.0099(9) 0.0005(8) 0.0047(8) C21 0.0271(10) 0.0296(10) 0.0302(10) 0.0002(9) 0.0088(8) -0.0070(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 Ru C21 1.855(2) . ? Ru C2 2.1653(18) . ? Ru C14 2.2071(18) . ? Ru C1 2.218(2) . ? Ru C15 2.219(2) . ? Ru C3 2.2204(17) . ? Ru C13 2.2344(18) . ? Ru C11 2.274(2) . ? Ru C12 2.2772(18) . ? O C21 1.159(3) . ? C1 C2 1.412(3) . ? C2 C3 1.435(3) . ? C2 C10 1.504(3) . ? C3 C4 1.485(2) . ? C4 C5 1.391(3) . ? C4 C9 1.401(3) . ? C5 C6 1.393(3) . ? C6 C7 1.394(4) . ? C7 C8 1.380(3) . ? C8 C9 1.392(3) . ? C11 C12 1.420(3) . ? C11 C15 1.435(3) . ? C11 C16 1.503(3) . ? C12 C13 1.434(3) . ? C12 C17 1.504(3) . ? C13 C14 1.425(3) . ? C13 C18 1.498(3) . ? C14 C15 1.434(3) . ? C14 C19 1.495(3) . ? C15 C20 1.507(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 C21 Ru C2 105.05(9) . . ? C21 Ru C14 90.67(8) . . ? C2 Ru C14 163.59(7) . . ? C21 Ru C1 86.32(9) . . ? C2 Ru C1 37.55(8) . . ? C14 Ru C1 142.28(7) . . ? C21 Ru C15 106.17(9) . . ? C2 Ru C15 136.82(8) . . ? C14 Ru C15 37.80(7) . . ? C1 Ru C15 167.24(8) . . ? C21 Ru C3 88.57(8) . . ? C2 Ru C3 38.16(7) . . ? C14 Ru C3 149.95(7) . . ? C1 Ru C3 67.63(7) . . ? C15 Ru C3 114.36(7) . . ? C21 Ru C13 111.57(8) . . ? C2 Ru C13 128.72(7) . . ? C14 Ru C13 37.41(7) . . ? C1 Ru C13 110.43(7) . . ? C15 Ru C13 63.00(7) . . ? C3 Ru C13 159.78(7) . . ? C21 Ru C11 143.20(9) . . ? C2 Ru C11 105.44(8) . . ? C14 Ru C11 61.95(7) . . ? C1 Ru C11 130.45(9) . . ? C15 Ru C11 37.21(9) . . ? C3 Ru C11 103.13(7) . . ? C13 Ru C11 61.92(7) . . ? C21 Ru C12 148.48(8) . . ? C2 Ru C12 101.94(7) . . ? C14 Ru C12 61.64(7) . . ? C1 Ru C12 106.05(7) . . ? C15 Ru C12 61.85(7) . . ? C3 Ru C12 122.90(7) . . ? C13 Ru C12 37.06(7) . . ? C11 Ru C12 36.36(7) . . ? C2 C1 Ru 69.18(11) . . ? C1 C2 C3 120.39(17) . . ? C1 C2 C10 119.69(17) . . ? C3 C2 C10 119.53(18) . . ? C1 C2 Ru 73.27(11) . . ? C3 C2 Ru 73.00(10) . . ? C10 C2 Ru 119.47(13) . . ? C2 C3 C4 126.26(17) . . ? C2 C3 Ru 68.83(10) . . ? C4 C3 Ru 116.52(12) . . ? C5 C4 C9 117.76(18) . . ? C5 C4 C3 123.04(16) . . ? C9 C4 C3 119.16(18) . . ? C4 C5 C6 121.7(2) . . ? C5 C6 C7 119.6(3) . . ? C8 C7 C6 119.5(2) . . ? C7 C8 C9 120.72(19) . . ? C8 C9 C4 120.7(2) . . ? C12 C11 C15 108.14(17) . . ? C12 C11 C16 126.66(19) . . ? C15 C11 C16 124.88(18) . . ? C12 C11 Ru 71.93(11) . . ? C15 C11 Ru 69.32(10) . . ? C16 C11 Ru 129.39(14) . . ? C11 C12 C13 108.72(16) . . ? C11 C12 C17 126.82(18) . . ? C13 C12 C17 124.11(18) . . ? C11 C12 Ru 71.71(11) . . ? C13 C12 Ru 69.85(9) . . ? C17 C12 Ru 129.66(14) . . ? C14 C13 C12 107.02(16) . . ? C14 C13 C18 127.07(17) . . ? C12 C13 C18 125.61(18) . . ? C14 C13 Ru 70.26(10) . . ? C12 C13 Ru 73.09(10) . . ? C18 C13 Ru 126.77(14) . . ? C13 C14 C15 109.00(16) . . ? C13 C14 C19 125.39(17) . . ? C15 C14 C19 125.34(18) . . ? C13 C14 Ru 72.34(10) . . ? C15 C14 Ru 71.57(11) . . ? C19 C14 Ru 126.98(14) . . ? C14 C15 C11 107.09(17) . . ? C14 C15 C20 125.8(2) . . ? C11 C15 C20 126.62(19) . . ? C14 C15 Ru 70.64(12) . . ? C11 C15 Ru 73.47(10) . . ? C20 C15 Ru 127.58(14) . . ? O C21 Ru 175.54(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Ru C1 C2 120.70(13) . . . . ? C14 Ru C1 C2 -152.96(12) . . . . ? C15 Ru C1 C2 -70.9(3) . . . . ? C3 Ru C1 C2 30.73(11) . . . . ? C13 Ru C1 C2 -127.63(11) . . . . ? C11 Ru C1 C2 -57.66(14) . . . . ? C12 Ru C1 C2 -88.80(12) . . . . ? Ru C1 C2 C3 -57.98(16) . . . . ? Ru C1 C2 C10 114.83(17) . . . . ? C21 Ru C2 C1 -62.70(14) . . . . ? C14 Ru C2 C1 100.2(3) . . . . ? C15 Ru C2 C1 162.24(12) . . . . ? C3 Ru C2 C1 -130.12(17) . . . . ? C13 Ru C2 C1 72.02(14) . . . . ? C11 Ru C2 C1 138.17(12) . . . . ? C12 Ru C2 C1 100.87(12) . . . . ? C21 Ru C2 C3 67.42(14) . . . . ? C14 Ru C2 C3 -129.7(3) . . . . ? C1 Ru C2 C3 130.12(17) . . . . ? C15 Ru C2 C3 -67.64(15) . . . . ? C13 Ru C2 C3 -157.86(12) . . . . ? C11 Ru C2 C3 -91.72(12) . . . . ? C12 Ru C2 C3 -129.01(12) . . . . ? C21 Ru C2 C10 -177.80(15) . . . . ? C14 Ru C2 C10 -14.9(4) . . . . ? C1 Ru C2 C10 -115.1(2) . . . . ? C15 Ru C2 C10 47.1(2) . . . . ? C3 Ru C2 C10 114.8(2) . . . . ? C13 Ru C2 C10 -43.1(2) . . . . ? C11 Ru C2 C10 23.07(17) . . . . ? C12 Ru C2 C10 -14.23(17) . . . . ? C1 C2 C3 C4 -49.9(3) . . . . ? C10 C2 C3 C4 137.25(19) . . . . ? Ru C2 C3 C4 -108.04(17) . . . . ? C1 C2 C3 Ru 58.11(17) . . . . ? C10 C2 C3 Ru -114.71(17) . . . . ? C21 Ru C3 C2 -116.88(14) . . . . ? C14 Ru C3 C2 154.25(14) . . . . ? C1 Ru C3 C2 -30.27(12) . . . . ? C15 Ru C3 C2 135.99(12) . . . . ? C13 Ru C3 C2 58.3(3) . . . . ? C11 Ru C3 C2 98.37(12) . . . . ? C12 Ru C3 C2 64.89(14) . . . . ? C21 Ru C3 C4 4.16(15) . . . . ? C2 Ru C3 C4 121.03(19) . . . . ? C14 Ru C3 C4 -84.7(2) . . . . ? C1 Ru C3 C4 90.77(14) . . . . ? C15 Ru C3 C4 -102.97(14) . . . . ? C13 Ru C3 C4 179.32(19) . . . . ? C11 Ru C3 C4 -140.59(13) . . . . ? C12 Ru C3 C4 -174.08(12) . . . . ? C2 C3 C4 C5 -8.2(3) . . . . ? Ru C3 C4 C5 -90.44(19) . . . . ? C2 C3 C4 C9 174.19(17) . . . . ? Ru C3 C4 C9 91.91(18) . . . . ? C9 C4 C5 C6 -3.0(3) . . . . ? C3 C4 C5 C6 179.28(18) . . . . ? C4 C5 C6 C7 2.7(3) . . . . ? C5 C6 C7 C8 -0.9(3) . . . . ? C6 C7 C8 C9 -0.4(3) . . . . ? C7 C8 C9 C4 0.0(3) . . . . ? C5 C4 C9 C8 1.7(3) . . . . ? C3 C4 C9 C8 179.46(17) . . . . ? C21 Ru C11 C12 125.78(15) . . . . ? C2 Ru C11 C12 -89.25(12) . . . . ? C14 Ru C11 C12 79.40(12) . . . . ? C1 Ru C11 C12 -56.96(14) . . . . ? C15 Ru C11 C12 118.25(18) . . . . ? C3 Ru C11 C12 -128.61(11) . . . . ? C13 Ru C11 C12 36.78(11) . . . . ? C21 Ru C11 C15 7.5(2) . . . . ? C2 Ru C11 C15 152.51(12) . . . . ? C14 Ru C11 C15 -38.85(11) . . . . ? C1 Ru C11 C15 -175.20(11) . . . . ? C3 Ru C11 C15 113.14(12) . . . . ? C13 Ru C11 C15 -81.47(13) . . . . ? C12 Ru C11 C15 -118.25(17) . . . . ? C21 Ru C11 C16 -111.2(2) . . . . ? C2 Ru C11 C16 33.8(2) . . . . ? C14 Ru C11 C16 -157.6(2) . . . . ? C1 Ru C11 C16 66.0(2) . . . . ? C15 Ru C11 C16 -118.8(2) . . . . ? C3 Ru C11 C16 -5.6(2) . . . . ? C13 Ru C11 C16 159.8(2) . . . . ? C12 Ru C11 C16 123.0(2) . . . . ? C15 C11 C12 C13 -0.2(2) . . . . ? C16 C11 C12 C13 173.57(19) . . . . ? Ru C11 C12 C13 -60.33(13) . . . . ? C15 C11 C12 C17 -173.54(19) . . . . ? C16 C11 C12 C17 0.2(3) . . . . ? Ru C11 C12 C17 126.3(2) . . . . ? C15 C11 C12 Ru 60.14(12) . . . . ? C16 C11 C12 Ru -126.1(2) . . . . ? C21 Ru C12 C11 -111.61(19) . . . . ? C2 Ru C12 C11 99.89(12) . . . . ? C14 Ru C12 C11 -80.32(12) . . . . ? C1 Ru C12 C11 138.41(12) . . . . ? C15 Ru C12 C11 -37.17(13) . . . . ? C3 Ru C12 C11 65.01(14) . . . . ? C13 Ru C12 C11 -118.77(17) . . . . ? C21 Ru C12 C13 7.2(2) . . . . ? C2 Ru C12 C13 -141.34(12) . . . . ? C14 Ru C12 C13 38.45(11) . . . . ? C1 Ru C12 C13 -102.81(13) . . . . ? C15 Ru C12 C13 81.60(13) . . . . ? C3 Ru C12 C13 -176.22(12) . . . . ? C11 Ru C12 C13 118.77(17) . . . . ? C21 Ru C12 C17 125.3(2) . . . . ? C2 Ru C12 C17 -23.19(19) . . . . ? C14 Ru C12 C17 156.6(2) . . . . ? C1 Ru C12 C17 15.33(19) . . . . ? C15 Ru C12 C17 -160.3(2) . . . . ? C3 Ru C12 C17 -58.1(2) . . . . ? C13 Ru C12 C17 118.1(2) . . . . ? C11 Ru C12 C17 -123.1(2) . . . . ? C11 C12 C13 C14 -1.0(2) . . . . ? C17 C12 C13 C14 172.61(19) . . . . ? Ru C12 C13 C14 -62.46(12) . . . . ? C11 C12 C13 C18 -175.02(18) . . . . ? C17 C12 C13 C18 -1.4(3) . . . . ? Ru C12 C13 C18 123.49(19) . . . . ? C11 C12 C13 Ru 61.49(13) . . . . ? C17 C12 C13 Ru -124.93(19) . . . . ? C21 Ru C13 C14 -60.25(14) . . . . ? C2 Ru C13 C14 167.30(12) . . . . ? C1 Ru C13 C14 -154.48(11) . . . . ? C15 Ru C13 C14 37.48(12) . . . . ? C3 Ru C13 C14 124.9(2) . . . . ? C11 Ru C13 C14 79.65(12) . . . . ? C12 Ru C13 C14 115.73(17) . . . . ? C21 Ru C13 C12 -175.98(13) . . . . ? C2 Ru C13 C12 51.57(15) . . . . ? C14 Ru C13 C12 -115.73(17) . . . . ? C1 Ru C13 C12 89.79(13) . . . . ? C15 Ru C13 C12 -78.25(13) . . . . ? C3 Ru C13 C12 9.2(3) . . . . ? C11 Ru C13 C12 -36.08(11) . . . . ? C21 Ru C13 C18 61.84(19) . . . . ? C2 Ru C13 C18 -70.6(2) . . . . ? C14 Ru C13 C18 122.1(2) . . . . ? C1 Ru C13 C18 -32.38(19) . . . . ? C15 Ru C13 C18 159.6(2) . . . . ? C3 Ru C13 C18 -113.0(3) . . . . ? C11 Ru C13 C18 -158.3(2) . . . . ? C12 Ru C13 C18 -122.2(2) . . . . ? C12 C13 C14 C15 1.8(2) . . . . ? C18 C13 C14 C15 175.70(18) . . . . ? Ru C13 C14 C15 -62.57(14) . . . . ? C12 C13 C14 C19 -172.42(18) . . . . ? C18 C13 C14 C19 1.5(3) . . . . ? Ru C13 C14 C19 123.24(19) . . . . ? C12 C13 C14 Ru 64.34(12) . . . . ? C18 C13 C14 Ru -121.73(19) . . . . ? C21 Ru C14 C13 126.15(13) . . . . ? C2 Ru C14 C13 -37.4(3) . . . . ? C1 Ru C14 C13 41.30(17) . . . . ? C15 Ru C14 C13 -117.79(16) . . . . ? C3 Ru C14 C13 -145.54(14) . . . . ? C11 Ru C14 C13 -79.55(12) . . . . ? C12 Ru C14 C13 -38.09(11) . . . . ? C21 Ru C14 C15 -116.06(13) . . . . ? C2 Ru C14 C15 80.4(3) . . . . ? C1 Ru C14 C15 159.09(13) . . . . ? C3 Ru C14 C15 -27.75(19) . . . . ? C13 Ru C14 C15 117.79(16) . . . . ? C11 Ru C14 C15 38.24(13) . . . . ? C12 Ru C14 C15 79.70(12) . . . . ? C21 Ru C14 C19 4.75(18) . . . . ? C2 Ru C14 C19 -158.8(2) . . . . ? C1 Ru C14 C19 -80.1(2) . . . . ? C15 Ru C14 C19 120.8(2) . . . . ? C3 Ru C14 C19 93.1(2) . . . . ? C13 Ru C14 C19 -121.4(2) . . . . ? C11 Ru C14 C19 159.05(19) . . . . ? C12 Ru C14 C19 -159.49(19) . . . . ? C13 C14 C15 C11 -1.9(2) . . . . ? C19 C14 C15 C11 172.31(18) . . . . ? Ru C14 C15 C11 -64.94(13) . . . . ? C13 C14 C15 C20 -174.02(19) . . . . ? C19 C14 C15 C20 0.2(3) . . . . ? Ru C14 C15 C20 122.9(2) . . . . ? C13 C14 C15 Ru 63.06(13) . . . . ? C19 C14 C15 Ru -122.75(19) . . . . ? C12 C11 C15 C14 1.3(2) . . . . ? C16 C11 C15 C14 -172.6(2) . . . . ? Ru C11 C15 C14 63.06(14) . . . . ? C12 C11 C15 C20 173.3(2) . . . . ? C16 C11 C15 C20 -0.6(3) . . . . ? Ru C11 C15 C20 -124.9(2) . . . . ? C12 C11 C15 Ru -61.80(13) . . . . ? C16 C11 C15 Ru 124.31(19) . . . . ? C21 Ru C15 C14 69.28(12) . . . . ? C2 Ru C15 C14 -155.97(11) . . . . ? C1 Ru C15 C14 -98.7(3) . . . . ? C3 Ru C15 C14 165.17(10) . . . . ? C13 Ru C15 C14 -37.10(10) . . . . ? C11 Ru C15 C14 -115.42(17) . . . . ? C12 Ru C15 C14 -79.10(11) . . . . ? C21 Ru C15 C11 -175.31(12) . . . . ? C2 Ru C15 C11 -40.56(17) . . . . ? C14 Ru C15 C11 115.42(17) . . . . ? C1 Ru C15 C11 16.7(4) . . . . ? C3 Ru C15 C11 -79.41(13) . . . . ? C13 Ru C15 C11 78.32(13) . . . . ? C12 Ru C15 C11 36.32(12) . . . . ? C21 Ru C15 C20 -51.5(2) . . . . ? C2 Ru C15 C20 83.3(2) . . . . ? C14 Ru C15 C20 -120.7(3) . . . . ? C1 Ru C15 C20 140.6(3) . . . . ? C3 Ru C15 C20 44.4(2) . . . . ? C13 Ru C15 C20 -157.8(2) . . . . ? C11 Ru C15 C20 123.8(2) . . . . ? C12 Ru C15 C20 160.2(2) . . . . ? C2 Ru C21 O -180(100) . . . . ? C14 Ru C21 O 5(3) . . . . ? C1 Ru C21 O 147(3) . . . . ? C15 Ru C21 O -30(3) . . . . ? C3 Ru C21 O -145(3) . . . . ? C13 Ru C21 O 37(3) . . . . ? C11 Ru C21 O -35(3) . . . . ? C12 Ru C21 O 32(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 72.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.319 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.056 #============================================================================= # end of cif data for "andyg35a" (compound 3) #============================================================================= #============================================================================= # end of cif file #=============================================================================