# Supplementary Material (ESI) for Green Chemistry # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full 'Green Chemistry' _journal_coden_Cambridge 1048 _publ_contact_author_name 'Pascale Crochet' _publ_contact_author_email CROCHETPASCALE@UNIOVI.ES _publ_section_title ; Highly water-soluble arene-ruthenium(II) complexes: application to catalytic isomerization of allylic alcohols in aqueous medium ; _publ_author_name 'Pascale Crochet' # Attachment 'Revised_CIF.cif' # Highly water-soluble arene-ruthenium(II)complexes: application to catalytic # isomerization of allylic alchols in aqueous medium. # Beatriz Lastra-BarreiraJosefina D\'iez,Pascale Crochet,* # Departamento de Qu\'imica Org\'anica e Inorg\'anica, Instituto Universitario # de Qu\'imica Organomet\'alica Enrique Moles (Unidad Asociada al CSIC), # Facultad de Qu\'imica, Universidad de Oviedo, E-33071 Oviedo, Spain. # Fax: (+34)-985 10 34 46. E-mail: pascale@fq.uniovi.es (P.C.). #=============================================================================== data_2a _database_code_depnum_ccdc_archive 'CCDC 728240' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H19 Cl2 O5 P Ru' _chemical_formula_sum 'C11 H19 Cl2 O5 P Ru' _chemical_formula_weight 434.20 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9850(6) _cell_length_b 7.3150(6) _cell_length_c 16.9400(16) _cell_angle_alpha 80.825(4) _cell_angle_beta 81.027(4) _cell_angle_gamma 63.636(5) _cell_volume 762.05(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2606 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.350 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.892 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 1.498 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.851 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95 mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9619 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 25.38 _reflns_number_total 2771 _reflns_number_gt 2286 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker, 2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowki & Minor 1997)' _computing_data_reduction 'HKL Denzo and scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2006)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0586P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2771 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4540(7) 0.9689(7) 0.0992(3) 0.0213(9) Uani 1 1 d . . . H1 H 0.3597 0.9956 0.0612 0.026 Uiso 1 1 calc R . . C2 C 0.4345(8) 1.1268(7) 0.1434(3) 0.0260(10) Uani 1 1 d . . . H2 H 0.3283 1.2588 0.1328 0.031 Uiso 1 1 calc R . . C3 C 0.5723(8) 1.0887(7) 0.2030(3) 0.0266(11) Uani 1 1 d . . . H3 H 0.5650 1.1948 0.2289 0.032 Uiso 1 1 calc R . . C4 C 0.7226(7) 0.8824(7) 0.2220(3) 0.0234(10) Uani 1 1 d . . . H4 H 0.8082 0.8530 0.2634 0.028 Uiso 1 1 calc R . . C5 C 0.7458(7) 0.7203(7) 0.1795(3) 0.0214(10) Uani 1 1 d . . . H5 H 0.8408 0.5856 0.1940 0.026 Uiso 1 1 calc R . . C6 C 0.6206(7) 0.7690(7) 0.1144(3) 0.0204(9) Uani 1 1 d . . . C7 C 0.7950(7) 0.4206(7) 0.0827(3) 0.0217(10) Uani 1 1 d . . . H7A H 0.7650 0.3643 0.1364 0.026 Uiso 1 1 calc R . . H7B H 0.9373 0.4157 0.0781 0.026 Uiso 1 1 calc R . . C8 C 0.7829(8) 0.2994(7) 0.0212(3) 0.0254(10) Uani 1 1 d . . . H8A H 0.8697 0.1545 0.0350 0.030 Uiso 1 1 calc R . . H8B H 0.6356 0.3203 0.0215 0.030 Uiso 1 1 calc R . . C9 C 0.7567(9) 0.4763(8) 0.3780(3) 0.0411(14) Uani 1 1 d . . . H9A H 0.6950 0.4641 0.3334 0.062 Uiso 1 1 calc R . . H9B H 0.7462 0.3807 0.4225 0.062 Uiso 1 1 calc R . . H9C H 0.9049 0.4470 0.3628 0.062 Uiso 1 1 calc R . . C10 C 0.0545(8) 0.7719(9) 0.4216(3) 0.0352(12) Uani 1 1 d . . . H10A H 0.0190 0.7732 0.3690 0.053 Uiso 1 1 calc R . . H10B H -0.0173 0.9081 0.4380 0.053 Uiso 1 1 calc R . . H10C H 0.0094 0.6819 0.4589 0.053 Uiso 1 1 calc R . . C11 C 0.3950(9) 1.1737(8) 0.3996(3) 0.0341(12) Uani 1 1 d . . . H11A H 0.5480 1.1173 0.3875 0.051 Uiso 1 1 calc R . . H11B H 0.3537 1.2559 0.4436 0.051 Uiso 1 1 calc R . . H11C H 0.3267 1.2574 0.3533 0.051 Uiso 1 1 calc R . . Cl1 Cl 0.29777(17) 0.61565(16) 0.23156(7) 0.0227(3) Uani 1 1 d . . . Cl2 Cl 0.03702(17) 1.11837(16) 0.25830(7) 0.0256(3) Uani 1 1 d . . . O1 O 0.6359(5) 0.6308(5) 0.06718(18) 0.0227(7) Uani 1 1 d . . . O2 O 0.8567(6) 0.3606(6) -0.0563(2) 0.0350(8) Uani 1 1 d . . . H2O H 0.9819 0.3411 -0.0567 0.053 Uiso 1 1 calc R . . O3 O 0.6415(5) 0.6838(5) 0.4013(2) 0.0332(8) Uani 1 1 d . . . O4 O 0.3298(6) 1.0089(5) 0.4214(2) 0.0355(8) Uani 1 1 d . . . O5 O 0.2841(6) 0.7004(6) 0.4201(2) 0.0349(8) Uani 1 1 d . . . P1 P 0.40998(18) 0.82246(18) 0.37042(7) 0.0199(3) Uani 1 1 d . . . Ru1 Ru 0.40797(5) 0.88443(5) 0.23334(2) 0.01669(14) 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 C1 0.023(2) 0.021(2) 0.014(2) 0.0018(17) 0.0011(18) -0.0054(19) C2 0.027(2) 0.018(2) 0.030(3) 0.0010(19) 0.008(2) -0.011(2) C3 0.031(3) 0.028(3) 0.029(3) -0.003(2) 0.003(2) -0.023(2) C4 0.023(2) 0.030(3) 0.022(2) -0.0031(19) 0.0005(19) -0.017(2) C5 0.010(2) 0.028(2) 0.025(2) -0.010(2) 0.0084(18) -0.0080(19) C6 0.019(2) 0.022(2) 0.021(2) -0.0045(18) 0.0041(18) -0.0099(19) C7 0.020(2) 0.021(2) 0.025(2) -0.0033(19) -0.0024(19) -0.0087(19) C8 0.027(2) 0.024(2) 0.029(3) -0.005(2) -0.001(2) -0.014(2) C9 0.041(3) 0.027(3) 0.039(3) -0.005(2) -0.012(3) 0.002(2) C10 0.026(3) 0.053(3) 0.032(3) -0.002(2) 0.002(2) -0.025(3) C11 0.043(3) 0.028(3) 0.035(3) -0.010(2) -0.005(2) -0.017(2) Cl1 0.0247(6) 0.0193(5) 0.0284(6) -0.0049(4) -0.0008(5) -0.0131(5) Cl2 0.0153(5) 0.0208(6) 0.0358(7) -0.0050(5) -0.0018(5) -0.0030(4) O1 0.0224(16) 0.0225(16) 0.0216(16) -0.0074(13) -0.0052(13) -0.0057(14) O2 0.037(2) 0.052(2) 0.0282(19) -0.0130(17) 0.0073(16) -0.0302(18) O3 0.0278(19) 0.033(2) 0.033(2) -0.0049(16) -0.0087(15) -0.0055(16) O4 0.041(2) 0.034(2) 0.031(2) -0.0114(16) 0.0004(16) -0.0148(17) O5 0.0306(19) 0.045(2) 0.031(2) -0.0013(16) -0.0010(15) -0.0193(17) P1 0.0183(6) 0.0231(6) 0.0185(6) -0.0032(5) -0.0021(5) -0.0085(5) Ru1 0.0155(2) 0.0158(2) 0.0193(2) -0.00337(14) -0.00140(14) -0.00672(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.421(6) . ? C1 C6 1.422(6) . ? C1 Ru1 2.269(4) . ? C1 H1 0.9300 . ? C2 C3 1.414(7) . ? C2 Ru1 2.201(4) . ? C2 H2 0.9300 . ? C3 C4 1.423(7) . ? C3 Ru1 2.216(4) . ? C3 H3 0.9300 . ? C4 C5 1.420(6) . ? C4 Ru1 2.170(4) . ? C4 H4 0.9300 . ? C5 C6 1.416(6) . ? C5 Ru1 2.237(4) . ? C5 H5 0.9300 . ? C6 O1 1.345(5) . ? C6 Ru1 2.340(4) . ? C7 O1 1.453(5) . ? C7 C8 1.505(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O2 1.414(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O3 1.454(6) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 O5 1.446(6) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O4 1.446(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? Cl1 Ru1 2.4145(10) . ? Cl2 Ru1 2.4024(11) . ? O2 H2O 0.8200 . ? O3 P1 1.598(3) . ? O4 P1 1.571(3) . ? O5 P1 1.583(4) . ? P1 Ru1 2.2948(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.6(4) . . ? C2 C1 Ru1 68.9(2) . . ? C6 C1 Ru1 74.8(2) . . ? C2 C1 H1 120.7 . . ? C6 C1 H1 120.7 . . ? Ru1 C1 H1 127.6 . . ? C3 C2 C1 121.7(4) . . ? C3 C2 Ru1 71.9(3) . . ? C1 C2 Ru1 74.1(2) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? Ru1 C2 H2 126.9 . . ? C2 C3 C4 117.8(4) . . ? C2 C3 Ru1 70.8(2) . . ? C4 C3 Ru1 69.3(2) . . ? C2 C3 H3 121.1 . . ? C4 C3 H3 121.1 . . ? Ru1 C3 H3 131.3 . . ? C5 C4 C3 121.9(4) . . ? C5 C4 Ru1 73.8(2) . . ? C3 C4 Ru1 72.8(3) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? Ru1 C4 H4 126.3 . . ? C6 C5 C4 118.3(4) . . ? C6 C5 Ru1 76.0(2) . . ? C4 C5 Ru1 68.7(2) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? Ru1 C5 H5 126.2 . . ? O1 C6 C5 123.9(4) . . ? O1 C6 C1 115.0(4) . . ? C5 C6 C1 120.9(4) . . ? O1 C6 Ru1 132.6(3) . . ? C5 C6 Ru1 68.1(2) . . ? C1 C6 Ru1 69.4(2) . . ? O1 C7 C8 107.3(4) . . ? O1 C7 H7A 110.3 . . ? C8 C7 H7A 110.3 . . ? O1 C7 H7B 110.3 . . ? C8 C7 H7B 110.3 . . ? H7A C7 H7B 108.5 . . ? O2 C8 C7 110.7(4) . . ? O2 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? O3 C9 H9A 109.5 . . ? O3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O5 C10 H10A 109.5 . . ? O5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O4 C11 H11A 109.5 . . ? O4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 O1 C7 117.8(3) . . ? C8 O2 H2O 109.5 . . ? C9 O3 P1 117.9(3) . . ? C11 O4 P1 122.7(3) . . ? C10 O5 P1 123.0(3) . . ? O4 P1 O5 100.2(2) . . ? O4 P1 O3 100.55(19) . . ? O5 P1 O3 98.90(19) . . ? O4 P1 Ru1 118.92(15) . . ? O5 P1 Ru1 119.90(14) . . ? O3 P1 Ru1 114.77(14) . . ? C4 Ru1 C2 67.53(18) . . ? C4 Ru1 C3 37.85(17) . . ? C2 Ru1 C3 37.34(17) . . ? C4 Ru1 C5 37.55(16) . . ? C2 Ru1 C5 79.41(17) . . ? C3 Ru1 C5 67.87(17) . . ? C4 Ru1 C1 79.07(17) . . ? C2 Ru1 C1 37.02(16) . . ? C3 Ru1 C1 67.00(17) . . ? C5 Ru1 C1 66.44(17) . . ? C4 Ru1 P1 90.56(12) . . ? C2 Ru1 P1 134.44(13) . . ? C3 Ru1 P1 102.18(13) . . ? C5 Ru1 P1 107.57(12) . . ? C1 Ru1 P1 168.81(12) . . ? C4 Ru1 C6 65.22(16) . . ? C2 Ru1 C6 65.04(16) . . ? C3 Ru1 C6 77.24(16) . . ? C5 Ru1 C6 35.95(16) . . ? C1 Ru1 C6 35.89(15) . . ? P1 Ru1 C6 141.68(11) . . ? C4 Ru1 Cl2 139.18(12) . . ? C2 Ru1 Cl2 86.29(13) . . ? C3 Ru1 Cl2 103.46(13) . . ? C5 Ru1 Cl2 164.77(13) . . ? C1 Ru1 Cl2 98.88(12) . . ? P1 Ru1 Cl2 86.18(4) . . ? C6 Ru1 Cl2 131.71(11) . . ? C4 Ru1 Cl1 131.89(12) . . ? C2 Ru1 Cl1 134.12(13) . . ? C3 Ru1 Cl1 162.73(13) . . ? C5 Ru1 Cl1 97.32(11) . . ? C1 Ru1 Cl1 99.50(12) . . ? P1 Ru1 Cl1 90.53(4) . . ? C6 Ru1 Cl1 85.53(10) . . ? Cl2 Ru1 Cl1 88.86(4) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.404 _refine_diff_density_min -1.146 _refine_diff_density_rms 0.137 #===END #=============================================================================== data_2b _database_code_depnum_ccdc_archive 'CCDC 728241' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H25 Cl2 O5 P Ru' _chemical_formula_sum 'C14 H25 Cl2 O5 P Ru' _chemical_formula_weight 476.28 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.6034(1) _cell_length_b 14.0769(2) _cell_length_c 18.3180(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.371(1) _cell_angle_gamma 90.00 _cell_volume 1849.63(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2971 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 25.350 _exptl_crystal_description Prismatic _exptl_crystal_colour Orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.71 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 1.242 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8012 _exptl_absorpt_correction_T_max 0.8856 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95 mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9264 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.23 _reflns_number_total 3301 _reflns_number_gt 2978 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker, 2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowki & Minor 1997)' _computing_data_reduction 'HKL Denzo and scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2006)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0659P)^2^+1.3467P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3301 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.1175 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.318 _refine_ls_restrained_S_all 1.318 _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 C1 C 0.4873(5) 0.2308(3) 1.06796(19) 0.0242(7) Uani 1 1 d . . . H1 H 0.3905 0.2451 1.0883 0.029 Uiso 1 1 calc R . . C2 C 0.5343(5) 0.1344(3) 1.05790(18) 0.0265(8) Uani 1 1 d . . . H2 H 0.4649 0.0848 1.0707 0.032 Uiso 1 1 calc R . . C3 C 0.6794(5) 0.1105(3) 1.0297(2) 0.0277(8) Uani 1 1 d . . . H3 H 0.7146 0.0461 1.0272 0.033 Uiso 1 1 calc R . . C4 C 0.7719(5) 0.1854(3) 1.0052(2) 0.0249(7) Uani 1 1 d . . . H4 H 0.8683 0.1711 0.9846 0.030 Uiso 1 1 calc R . . C5 C 0.7218(5) 0.2803(3) 1.0111(2) 0.0237(7) Uani 1 1 d . . . H5 H 0.7778 0.3295 0.9909 0.028 Uiso 1 1 calc R . . C6 C 0.5872(5) 0.3037(2) 1.0472(2) 0.0222(7) Uani 1 1 d . . . C7 C 0.4198(5) 0.4325(3) 1.0841(2) 0.0286(8) Uani 1 1 d . . . H7A H 0.4614 0.4947 1.1091 0.034 Uiso 1 1 calc R . . H7B H 0.4099 0.3881 1.1245 0.034 Uiso 1 1 calc R . . C8 C 0.2310(5) 0.4439(3) 1.0238(2) 0.0328(8) Uani 1 1 d . . . H8A H 0.1565 0.4880 1.0439 0.039 Uiso 1 1 calc R . . H8B H 0.2466 0.4736 0.9774 0.039 Uiso 1 1 calc R . . C9 C 0.7377(5) 0.2677(3) 0.8189(2) 0.0299(8) Uani 1 1 d . . . H9A H 0.8466 0.2326 0.8533 0.036 Uiso 1 1 calc R . . H9B H 0.6988 0.3151 0.8505 0.036 Uiso 1 1 calc R . . C10 C 0.7890(6) 0.3165(3) 0.7565(2) 0.0355(9) Uani 1 1 d . . . H10A H 0.8159 0.2689 0.7226 0.053 Uiso 1 1 calc R . . H10B H 0.8995 0.3561 0.7797 0.053 Uiso 1 1 calc R . . H10C H 0.6850 0.3566 0.7261 0.053 Uiso 1 1 calc R . . C11 C 0.6913(5) -0.0107(3) 0.8015(2) 0.0363(9) Uani 1 1 d . . . H11A H 0.7322 0.0312 0.7668 0.044 Uiso 1 1 calc R . . H11B H 0.5803 -0.0466 0.7698 0.044 Uiso 1 1 calc R . . C12 C 0.8428(5) -0.0774(3) 0.8420(2) 0.0329(8) Uani 1 1 d . . . H12A H 0.9525 -0.0413 0.8730 0.049 Uiso 1 1 calc R . . H12B H 0.8753 -0.1160 0.8039 0.049 Uiso 1 1 calc R . . H12C H 0.8010 -0.1188 0.8760 0.049 Uiso 1 1 calc R . . C13 C 0.1726(5) 0.1442(3) 0.7273(2) 0.0289(8) Uani 1 1 d . . . H13A H 0.1997 0.1828 0.6872 0.035 Uiso 1 1 calc R . . H13B H 0.1363 0.1874 0.7625 0.035 Uiso 1 1 calc R . . C14 C 0.0196(5) 0.0756(3) 0.6907(3) 0.0403(10) Uani 1 1 d . . . H14A H 0.0553 0.0348 0.6546 0.060 Uiso 1 1 calc R . . H14B H -0.0942 0.1106 0.6625 0.060 Uiso 1 1 calc R . . H14C H -0.0032 0.0364 0.7308 0.060 Uiso 1 1 calc R . . O1 O 0.5590(3) 0.39688(17) 1.05246(13) 0.0237(5) Uani 1 1 d . . . O2 O 0.1295(4) 0.3578(2) 1.00144(17) 0.0362(6) Uani 1 1 d . . . H2O H 0.0257 0.3694 0.9679 0.054 Uiso 1 1 calc R . . O3 O 0.5846(4) 0.20184(16) 0.78324(15) 0.0256(6) Uani 1 1 d . . . O4 O 0.6445(3) 0.04635(17) 0.85919(13) 0.0236(5) Uani 1 1 d . . . O5 O 0.3362(3) 0.08892(17) 0.77053(14) 0.0253(5) Uani 1 1 d . . . P1 P 0.50690(11) 0.13459(6) 0.83586(5) 0.0206(2) Uani 1 1 d . . . Cl1 Cl 0.32330(11) 0.33320(6) 0.86621(5) 0.0259(2) Uani 1 1 d . . . Cl2 Cl 0.16843(11) 0.12895(6) 0.91330(5) 0.0270(2) Uani 1 1 d . . . Ru1 Ru 0.47293(3) 0.199246(18) 0.944425(14) 0.01859(15) 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 C1 0.0278(17) 0.0290(19) 0.0164(16) 0.0017(14) 0.0079(14) -0.0024(15) C2 0.036(2) 0.0230(19) 0.0174(17) 0.0033(12) 0.0043(15) -0.0011(13) C3 0.0284(18) 0.0257(18) 0.0224(17) 0.0016(14) -0.0006(14) 0.0062(14) C4 0.0201(16) 0.0294(18) 0.0206(17) -0.0034(14) 0.0004(13) 0.0018(13) C5 0.0212(17) 0.0269(17) 0.0218(17) -0.0005(14) 0.0053(13) -0.0025(14) C6 0.0238(17) 0.0216(19) 0.0180(17) -0.0015(12) 0.0027(14) -0.0035(12) C7 0.0325(18) 0.0257(18) 0.034(2) -0.0053(15) 0.0198(16) -0.0031(15) C8 0.0315(19) 0.0284(19) 0.044(2) 0.0004(17) 0.0204(17) -0.0026(15) C9 0.0254(18) 0.0302(19) 0.0299(19) 0.0038(16) 0.0035(14) -0.0060(15) C10 0.034(2) 0.042(2) 0.032(2) -0.0011(17) 0.0119(17) -0.0086(17) C11 0.037(2) 0.044(2) 0.029(2) -0.0035(17) 0.0129(16) 0.0149(18) C12 0.0321(19) 0.0285(19) 0.039(2) -0.0036(16) 0.0129(16) 0.0056(15) C13 0.0228(17) 0.035(2) 0.0265(18) 0.0009(15) 0.0055(14) 0.0045(15) C14 0.0226(18) 0.046(2) 0.044(2) 0.0015(19) 0.0003(16) -0.0004(17) O1 0.0260(12) 0.0208(13) 0.0266(13) -0.0029(9) 0.0119(10) -0.0024(9) O2 0.0257(13) 0.0387(15) 0.0464(16) -0.0031(13) 0.0148(12) -0.0049(11) O3 0.0240(13) 0.0312(15) 0.0223(13) 0.0004(9) 0.0085(10) -0.0045(9) O4 0.0238(11) 0.0261(12) 0.0209(11) -0.0011(9) 0.0075(9) 0.0043(9) O5 0.0213(11) 0.0260(13) 0.0267(12) -0.0031(10) 0.0056(10) 0.0013(9) P1 0.0185(4) 0.0222(5) 0.0209(4) 0.0005(3) 0.0061(3) 0.0004(3) Cl1 0.0280(4) 0.0213(4) 0.0255(4) 0.0035(3) 0.0050(3) 0.0031(3) Cl2 0.0194(4) 0.0280(5) 0.0334(5) 0.0011(3) 0.0084(3) -0.0026(3) Ru1 0.0180(2) 0.0176(2) 0.0198(2) 0.00091(9) 0.00578(14) 0.00051(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.402(5) . ? C1 C2 1.431(5) . ? C1 Ru1 2.273(3) . ? C1 H1 0.9500 . ? C2 C3 1.405(5) . ? C2 Ru1 2.175(3) . ? C2 H2 0.9500 . ? C3 C4 1.422(5) . ? C3 Ru1 2.200(3) . ? C3 H3 0.9500 . ? C4 C5 1.404(5) . ? C4 Ru1 2.183(3) . ? C4 H4 0.9500 . ? C5 C6 1.429(5) . ? C5 Ru1 2.200(3) . ? C5 H5 0.9500 . ? C6 O1 1.338(4) . ? C6 Ru1 2.319(3) . ? C7 O1 1.455(4) . ? C7 C8 1.501(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O2 1.423(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O3 1.462(4) . ? C9 C10 1.493(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 O4 1.461(4) . ? C11 C12 1.480(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O5 1.458(4) . ? C13 C14 1.489(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O2 H2O 0.8400 . ? O3 P1 1.598(3) . ? O4 P1 1.589(2) . ? O5 P1 1.581(2) . ? P1 Ru1 2.2783(9) . ? Cl1 Ru1 2.4129(8) . ? Cl2 Ru1 2.4060(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.6(3) . . ? C6 C1 Ru1 74.0(2) . . ? C2 C1 Ru1 67.55(18) . . ? C6 C1 H1 120.7 . . ? C2 C1 H1 120.7 . . ? Ru1 C1 H1 130.1 . . ? C3 C2 C1 122.3(3) . . ? C3 C2 Ru1 72.25(19) . . ? C1 C2 Ru1 74.99(19) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? Ru1 C2 H2 125.7 . . ? C2 C3 C4 118.0(3) . . ? C2 C3 Ru1 70.29(19) . . ? C4 C3 Ru1 70.4(2) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? Ru1 C3 H3 130.8 . . ? C5 C4 C3 120.4(3) . . ? C5 C4 Ru1 72.0(2) . . ? C3 C4 Ru1 71.73(19) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? Ru1 C4 H4 128.8 . . ? C4 C5 C6 120.6(3) . . ? C4 C5 Ru1 70.7(2) . . ? C6 C5 Ru1 76.1(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? Ru1 C5 H5 125.2 . . ? O1 C6 C1 125.8(3) . . ? O1 C6 C5 114.5(3) . . ? C1 C6 C5 119.5(3) . . ? O1 C6 Ru1 130.8(2) . . ? C1 C6 Ru1 70.4(2) . . ? C5 C6 Ru1 67.10(19) . . ? O1 C7 C8 112.9(3) . . ? O1 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? O1 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? O2 C8 C7 114.6(3) . . ? O2 C8 H8A 108.6 . . ? C7 C8 H8A 108.6 . . ? O2 C8 H8B 108.6 . . ? C7 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? O3 C9 C10 108.7(3) . . ? O3 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? O3 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.3 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O4 C11 C12 108.8(3) . . ? O4 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? O4 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O5 C13 C14 107.3(3) . . ? O5 C13 H13A 110.3 . . ? C14 C13 H13A 110.3 . . ? O5 C13 H13B 110.3 . . ? C14 C13 H13B 110.3 . . ? H13A C13 H13B 108.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C6 O1 C7 121.4(3) . . ? C8 O2 H2O 109.5 . . ? C9 O3 P1 120.3(2) . . ? C11 O4 P1 122.1(2) . . ? C13 O5 P1 122.2(2) . . ? O5 P1 O4 100.82(13) . . ? O5 P1 O3 99.17(13) . . ? O4 P1 O3 106.44(13) . . ? O5 P1 Ru1 121.40(10) . . ? O4 P1 Ru1 109.44(9) . . ? O3 P1 Ru1 117.49(10) . . ? C2 Ru1 C4 67.57(14) . . ? C2 Ru1 C3 37.46(13) . . ? C4 Ru1 C3 37.84(14) . . ? C2 Ru1 C5 79.35(14) . . ? C4 Ru1 C5 37.35(13) . . ? C3 Ru1 C5 67.73(14) . . ? C2 Ru1 C1 37.46(13) . . ? C4 Ru1 C1 79.15(13) . . ? C3 Ru1 C1 67.44(13) . . ? C5 Ru1 C1 66.26(13) . . ? C2 Ru1 P1 128.03(11) . . ? C4 Ru1 P1 90.51(10) . . ? C3 Ru1 P1 97.61(10) . . ? C5 Ru1 P1 111.48(9) . . ? C1 Ru1 P1 164.83(10) . . ? C2 Ru1 C6 65.56(13) . . ? C4 Ru1 C6 66.20(13) . . ? C3 Ru1 C6 78.26(13) . . ? C5 Ru1 C6 36.76(13) . . ? C1 Ru1 C6 35.52(13) . . ? P1 Ru1 C6 147.33(10) . . ? C2 Ru1 Cl2 86.45(10) . . ? C4 Ru1 Cl2 147.30(10) . . ? C3 Ru1 Cl2 109.78(10) . . ? C5 Ru1 Cl2 158.06(10) . . ? C1 Ru1 Cl2 92.36(9) . . ? P1 Ru1 Cl2 90.44(3) . . ? C6 Ru1 Cl2 121.67(10) . . ? C2 Ru1 Cl1 143.63(10) . . ? C4 Ru1 Cl1 125.36(10) . . ? C3 Ru1 Cl1 161.90(10) . . ? C5 Ru1 Cl1 94.21(10) . . ? C1 Ru1 Cl1 107.22(10) . . ? P1 Ru1 Cl1 87.79(3) . . ? C6 Ru1 Cl1 87.86(9) . . ? Cl2 Ru1 Cl1 87.34(3) . . ? 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 C6 C1 C2 C3 1.5(5) . . . . ? Ru1 C1 C2 C3 57.1(3) . . . . ? C6 C1 C2 Ru1 -55.6(3) . . . . ? C1 C2 C3 C4 -4.9(5) . . . . ? Ru1 C2 C3 C4 53.6(3) . . . . ? C1 C2 C3 Ru1 -58.4(3) . . . . ? C2 C3 C4 C5 1.6(5) . . . . ? Ru1 C3 C4 C5 55.1(3) . . . . ? C2 C3 C4 Ru1 -53.5(3) . . . . ? C3 C4 C5 C6 4.8(5) . . . . ? Ru1 C4 C5 C6 59.8(3) . . . . ? C3 C4 C5 Ru1 -55.0(3) . . . . ? C2 C1 C6 O1 179.3(3) . . . . ? Ru1 C1 C6 O1 126.8(3) . . . . ? C2 C1 C6 C5 5.0(5) . . . . ? Ru1 C1 C6 C5 -47.5(3) . . . . ? C2 C1 C6 Ru1 52.5(3) . . . . ? C4 C5 C6 O1 176.8(3) . . . . ? Ru1 C5 C6 O1 -126.0(3) . . . . ? C4 C5 C6 C1 -8.2(5) . . . . ? Ru1 C5 C6 C1 49.0(3) . . . . ? C4 C5 C6 Ru1 -57.2(3) . . . . ? O1 C7 C8 O2 78.1(4) . . . . ? C1 C6 O1 C7 2.2(5) . . . . ? C5 C6 O1 C7 176.8(3) . . . . ? Ru1 C6 O1 C7 96.7(4) . . . . ? C8 C7 O1 C6 -89.0(4) . . . . ? C10 C9 O3 P1 176.5(3) . . . . ? C12 C11 O4 P1 171.5(3) . . . . ? C14 C13 O5 P1 -162.0(3) . . . . ? C13 O5 P1 O4 -177.1(2) . . . . ? C13 O5 P1 O3 -68.3(3) . . . . ? C13 O5 P1 Ru1 61.9(3) . . . . ? C11 O4 P1 O5 50.0(3) . . . . ? C11 O4 P1 O3 -53.1(3) . . . . ? C11 O4 P1 Ru1 179.0(2) . . . . ? C9 O3 P1 O5 174.3(3) . . . . ? C9 O3 P1 O4 -81.5(3) . . . . ? C9 O3 P1 Ru1 41.5(3) . . . . ? C3 C2 Ru1 C4 -30.0(2) . . . . ? C1 C2 Ru1 C4 101.8(2) . . . . ? C1 C2 Ru1 C3 131.8(3) . . . . ? C3 C2 Ru1 C5 -67.1(2) . . . . ? C1 C2 Ru1 C5 64.7(2) . . . . ? C3 C2 Ru1 C1 -131.8(3) . . . . ? C3 C2 Ru1 P1 41.9(3) . . . . ? C1 C2 Ru1 P1 173.67(16) . . . . ? C3 C2 Ru1 C6 -103.0(2) . . . . ? C1 C2 Ru1 C6 28.7(2) . . . . ? C3 C2 Ru1 Cl2 129.7(2) . . . . ? C1 C2 Ru1 Cl2 -98.55(19) . . . . ? C3 C2 Ru1 Cl1 -149.69(18) . . . . ? C1 C2 Ru1 Cl1 -17.9(3) . . . . ? C5 C4 Ru1 C2 -102.2(2) . . . . ? C3 C4 Ru1 C2 29.7(2) . . . . ? C5 C4 Ru1 C3 -131.9(3) . . . . ? C3 C4 Ru1 C5 131.9(3) . . . . ? C5 C4 Ru1 C1 -64.9(2) . . . . ? C3 C4 Ru1 C1 67.0(2) . . . . ? C5 C4 Ru1 P1 126.3(2) . . . . ? C3 C4 Ru1 P1 -101.8(2) . . . . ? C5 C4 Ru1 C6 -30.1(2) . . . . ? C3 C4 Ru1 C6 101.8(2) . . . . ? C5 C4 Ru1 Cl2 -142.11(18) . . . . ? C3 C4 Ru1 Cl2 -10.2(3) . . . . ? C5 C4 Ru1 Cl1 38.6(2) . . . . ? C3 C4 Ru1 Cl1 170.55(17) . . . . ? C4 C3 Ru1 C2 -131.1(3) . . . . ? C2 C3 Ru1 C4 131.1(3) . . . . ? C2 C3 Ru1 C5 101.9(2) . . . . ? C4 C3 Ru1 C5 -29.2(2) . . . . ? C2 C3 Ru1 C1 29.4(2) . . . . ? C4 C3 Ru1 C1 -101.7(2) . . . . ? C2 C3 Ru1 P1 -148.0(2) . . . . ? C4 C3 Ru1 P1 80.9(2) . . . . ? C2 C3 Ru1 C6 64.9(2) . . . . ? C4 C3 Ru1 C6 -66.2(2) . . . . ? C2 C3 Ru1 Cl2 -54.7(2) . . . . ? C4 C3 Ru1 Cl2 174.17(18) . . . . ? C2 C3 Ru1 Cl1 105.6(3) . . . . ? C4 C3 Ru1 Cl1 -25.5(4) . . . . ? C4 C5 Ru1 C2 66.8(2) . . . . ? C6 C5 Ru1 C2 -63.1(2) . . . . ? C6 C5 Ru1 C4 -130.0(3) . . . . ? C4 C5 Ru1 C3 29.6(2) . . . . ? C6 C5 Ru1 C3 -100.4(2) . . . . ? C4 C5 Ru1 C1 103.7(2) . . . . ? C6 C5 Ru1 C1 -26.2(2) . . . . ? C4 C5 Ru1 P1 -60.0(2) . . . . ? C6 C5 Ru1 P1 170.01(17) . . . . ? C4 C5 Ru1 C6 130.0(3) . . . . ? C4 C5 Ru1 Cl2 117.4(3) . . . . ? C6 C5 Ru1 Cl2 -12.6(4) . . . . ? C4 C5 Ru1 Cl1 -149.3(2) . . . . ? C6 C5 Ru1 Cl1 80.73(19) . . . . ? C6 C1 Ru1 C2 131.1(3) . . . . ? C6 C1 Ru1 C4 64.0(2) . . . . ? C2 C1 Ru1 C4 -67.1(2) . . . . ? C6 C1 Ru1 C3 101.7(2) . . . . ? C2 C1 Ru1 C3 -29.4(2) . . . . ? C6 C1 Ru1 C5 27.1(2) . . . . ? C2 C1 Ru1 C5 -104.0(2) . . . . ? C6 C1 Ru1 P1 111.7(4) . . . . ? C2 C1 Ru1 P1 -19.4(5) . . . . ? C2 C1 Ru1 C6 -131.1(3) . . . . ? C6 C1 Ru1 Cl2 -147.8(2) . . . . ? C2 C1 Ru1 Cl2 81.06(19) . . . . ? C6 C1 Ru1 Cl1 -59.9(2) . . . . ? C2 C1 Ru1 Cl1 169.00(18) . . . . ? O5 P1 Ru1 C2 98.01(17) . . . . ? O4 P1 Ru1 C2 -18.65(17) . . . . ? O3 P1 Ru1 C2 -140.11(16) . . . . ? O5 P1 Ru1 C4 159.49(15) . . . . ? O4 P1 Ru1 C4 42.83(14) . . . . ? O3 P1 Ru1 C4 -78.64(15) . . . . ? O5 P1 Ru1 C3 122.19(15) . . . . ? O4 P1 Ru1 C3 5.54(14) . . . . ? O3 P1 Ru1 C3 -115.93(15) . . . . ? O5 P1 Ru1 C5 -168.81(15) . . . . ? O4 P1 Ru1 C5 74.54(14) . . . . ? O3 P1 Ru1 C5 -46.93(15) . . . . ? O5 P1 Ru1 C1 112.9(4) . . . . ? O4 P1 Ru1 C1 -3.8(4) . . . . ? O3 P1 Ru1 C1 -125.3(4) . . . . ? O5 P1 Ru1 C6 -157.72(19) . . . . ? O4 P1 Ru1 C6 85.63(19) . . . . ? O3 P1 Ru1 C6 -35.8(2) . . . . ? O5 P1 Ru1 Cl2 12.17(12) . . . . ? O4 P1 Ru1 Cl2 -104.49(10) . . . . ? O3 P1 Ru1 Cl2 134.05(11) . . . . ? O5 P1 Ru1 Cl1 -75.15(12) . . . . ? O4 P1 Ru1 Cl1 168.19(10) . . . . ? O3 P1 Ru1 Cl1 46.73(11) . . . . ? O1 C6 Ru1 C2 -151.1(4) . . . . ? C1 C6 Ru1 C2 -30.2(2) . . . . ? C5 C6 Ru1 C2 105.6(2) . . . . ? O1 C6 Ru1 C4 133.8(4) . . . . ? C1 C6 Ru1 C4 -105.3(2) . . . . ? C5 C6 Ru1 C4 30.5(2) . . . . ? O1 C6 Ru1 C3 171.7(4) . . . . ? C1 C6 Ru1 C3 -67.5(2) . . . . ? C5 C6 Ru1 C3 68.4(2) . . . . ? O1 C6 Ru1 C5 103.3(4) . . . . ? C1 C6 Ru1 C5 -135.8(3) . . . . ? O1 C6 Ru1 C1 -120.9(4) . . . . ? C5 C6 Ru1 C1 135.8(3) . . . . ? O1 C6 Ru1 P1 85.9(4) . . . . ? C1 C6 Ru1 P1 -153.24(18) . . . . ? C5 C6 Ru1 P1 -17.4(3) . . . . ? O1 C6 Ru1 Cl2 -82.2(3) . . . . ? C1 C6 Ru1 Cl2 38.7(2) . . . . ? C5 C6 Ru1 Cl2 174.50(17) . . . . ? O1 C6 Ru1 Cl1 3.3(3) . . . . ? C1 C6 Ru1 Cl1 124.2(2) . . . . ? C5 C6 Ru1 Cl1 -99.95(19) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.23 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.298 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.227 #===END