data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Tiziana Funaioli' _publ_contact_author_address ; Chimica e Chimica Industriale Universita di Pisa Via Risorgimento 35 Pisa 56126 ITALY ; _publ_contact_author_phone 39()0502219255 _publ_contact_author_fax 39()0502219260 _publ_contact_author_email tiziana@dcci.unipi.it #============================================================================ # 3. TITLE AND AUTHOR LIST _publ_section_title ; The Ethene Hydroformylation with CO/H~2~O: Nucleophilic Attack by Water onto a Terminal CO of a Ru(II) Acylcarbonyl Complex ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address G.Fachinetti ; Dipartimento di Chimica e Chimica Industriale Universita di Pisa Via Risorgimento, 35 56126 Pisa Italy ; T.Funaioli ; Dipartimento di Chimica e Chimica Industriale Universita di Pisa Via Risorgimento, 35 56126 Pisa Italy ; F.Marchetti ; Dipartimento di Chimica e Chimica Industriale Universita di Pisa Via Risorgimento, 35 56126 Pisa Italy ; data_ruschif _database_code_depnum_ccdc_archive 'CCDC 211423' _audit_creation_method SHELXL-97 _chemical_name_systematic ; disodium bis-propionyldipropionatedicarbonyl-ruthenate(ii) ; _chemical_name_common 'disodium bis-propionyldipropionatedicarbonyl-ruthenate(ii)' _chemical_melting_point ? _chemical_formula_moiety '2(C11 H15 O7 Ru), 2Na' _chemical_formula_sum 'C22 H30 Na2 O14 Ru2' _chemical_formula_weight 766.58 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' Na Na 0.0362 0.0249 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.672(6) _cell_length_b 12.450(4) _cell_length_c 14.069(6) _cell_angle_alpha 73.26(3) _cell_angle_beta 75.03(4) _cell_angle_gamma 65.11(3) _cell_volume 1603.6(12) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 5.230 _cell_measurement_theta_max 19.381 _exptl_crystal_description 'Flattened prism (100)' _exptl_crystal_colour 'Light green (colourless?)' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.912 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4947 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.1073 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4143 _reflns_number_gt 2365 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'WINGX-1.64 (Farrugia, 2001)' _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^)+(0.0733P)^2^+11.2221P] 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 4143 _refine_ls_number_parameters 358 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1459 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.2174 _refine_ls_wR_factor_gt 0.1850 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.15642(15) 0.26463(11) 0.37770(10) 0.0516(4) Uani 1 1 d . A . C1 C 0.260(2) 0.1001(16) 0.4114(13) 0.076(6) Uani 1 1 d . . . O1 O 0.3222(15) -0.0006(11) 0.4305(10) 0.098(4) Uani 1 1 d . . . C2 C 0.256(2) 0.2609(14) 0.2515(15) 0.078(6) Uani 1 1 d . . . O2 O 0.3293(18) 0.2567(13) 0.1725(11) 0.109(5) Uani 1 1 d . . . O3 O 0.0342(11) 0.2784(9) 0.5190(7) 0.053(3) Uani 1 1 d . . . O4 O -0.0111(12) 0.1131(9) 0.5335(8) 0.066(3) Uani 1 1 d . . . C3 C -0.0301(18) 0.2081(15) 0.5630(12) 0.059(4) Uani 1 1 d . . . C4 C -0.133(2) 0.2344(19) 0.6585(13) 0.079(5) Uani 1 1 d . . . H4A H -0.1282 0.1587 0.7052 0.095 Uiso 1 1 calc R . . H4B H -0.1078 0.2806 0.6899 0.095 Uiso 1 1 calc R . . C5 C -0.280(2) 0.304(2) 0.6371(18) 0.122(8) Uani 1 1 d . . . H5A H -0.3422 0.3206 0.6985 0.182 Uiso 1 1 calc R . . H5B H -0.3067 0.2568 0.6084 0.182 Uiso 1 1 calc R . . H5C H -0.2852 0.3786 0.5906 0.182 Uiso 1 1 calc R . . O5 O 0.0078(13) 0.4468(9) 0.3425(8) 0.067(3) Uani 1 1 d . . . O6 O -0.0602(13) 0.3062(9) 0.3357(8) 0.072(3) Uani 1 1 d . A . C6 C -0.088(2) 0.4170(16) 0.3341(13) 0.068(5) Uani 1 1 d . . . C7 C -0.233(2) 0.5123(17) 0.3179(17) 0.098(7) Uani 1 1 d . . . H7A H -0.2857 0.4755 0.3000 0.117 Uiso 1 1 calc R . . H7B H -0.2821 0.5384 0.3806 0.117 Uiso 1 1 calc R . . C8 C -0.230(3) 0.617(2) 0.240(3) 0.184(15) Uani 1 1 d . . . H8A H -0.3237 0.6730 0.2335 0.277 Uiso 1 1 calc R . . H8B H -0.1828 0.5924 0.1777 0.277 Uiso 1 1 calc R . . H8C H -0.1806 0.6558 0.2584 0.277 Uiso 1 1 calc R . . C9 C 0.2930(17) 0.3066(13) 0.4173(12) 0.059(4) Uani 1 1 d . . . O7 O 0.2377(12) 0.3965(10) 0.4586(10) 0.079(4) Uani 1 1 d . . . C10 C 0.4489(18) 0.2454(17) 0.4015(17) 0.085(6) Uani 1 1 d . . . H10A H 0.4817 0.2496 0.3300 0.102 Uiso 1 1 calc R . . H10B H 0.4729 0.1606 0.4335 0.102 Uiso 1 1 calc R . . C11 C 0.5281(19) 0.2970(19) 0.4414(18) 0.100(7) Uani 1 1 d . . . H11A H 0.6267 0.2515 0.4282 0.150 Uiso 1 1 calc R . . H11B H 0.4985 0.2916 0.5125 0.150 Uiso 1 1 calc R . . H11C H 0.5085 0.3801 0.4085 0.150 Uiso 1 1 calc R . . Ru2 Ru -0.0826(2) 0.22184(13) 0.11120(11) 0.0915(7) Uani 1 1 d . A . C12 C -0.258(4) 0.329(2) 0.159(2) 0.115(9) Uani 1 1 d . . . O8 O -0.362(3) 0.392(2) 0.1897(18) 0.172(10) Uani 1 1 d . . . C13 C -0.009(3) 0.3334(19) 0.0921(16) 0.095(7) Uani 1 1 d . . . O9 O 0.045(2) 0.4017(17) 0.0832(15) 0.164(9) Uani 1 1 d . . . O10 O 0.118(2) 0.0878(12) 0.0659(11) 0.123(6) Uani 1 1 d . . . O11 O 0.1132(14) 0.0835(10) 0.2213(9) 0.078(4) Uani 1 1 d . A . C14 C 0.176(2) 0.0468(15) 0.1414(17) 0.073(5) Uani 1 1 d . . . C15 C 0.331(3) -0.045(2) 0.146(2) 0.147(12) Uani 1 1 d D . . H15A H 0.3890 -0.0012 0.1440 0.176 Uiso 1 1 calc R . . H15B H 0.3350 -0.1034 0.2089 0.176 Uiso 1 1 calc R . . C16 C 0.386(4) -0.108(4) 0.062(3) 0.25(2) Uani 1 1 d D . . H16A H 0.4809 -0.1635 0.0678 0.381 Uiso 1 1 calc R . . H16B H 0.3850 -0.0504 0.0000 0.381 Uiso 1 1 calc R . . H16C H 0.3299 -0.1519 0.0646 0.381 Uiso 1 1 calc R . . O12 O -0.152(2) 0.0816(12) 0.1363(10) 0.126(7) Uani 1 1 d . A . O13 O -0.1931(14) 0.0838(11) 0.2938(9) 0.086(4) Uani 1 1 d . A . C17 C -0.1919(19) 0.0428(16) 0.2232(14) 0.066(5) Uani 1 1 d . . . C18A C -0.251(4) -0.053(4) 0.222(2) 0.093(9) Uiso 0.56(2) 1 d PG A 1 H18A H -0.1399 -0.0896 0.2223 0.121 Uiso 0.56(2) 1 calc PG A 1 H18B H -0.2705 -0.0878 0.1674 0.121 Uiso 0.56(2) 1 calc PG A 1 C19A C -0.326(4) -0.091(3) 0.325(2) 0.093(9) Uiso 0.56(2) 1 d PG A 1 H19A H -0.2882 -0.1888 0.3454 0.121 Uiso 0.56(2) 1 calc PG A 1 H19B H -0.3052 -0.0571 0.3794 0.121 Uiso 0.56(2) 1 calc PG A 1 H19C H -0.4369 -0.0552 0.3241 0.121 Uiso 0.56(2) 1 calc PG A 1 C18B C -0.237(4) -0.070(5) 0.266(4) 0.093(9) Uiso 0.44(2) 1 d PG A 2 H18C H -0.2277 -0.1379 0.3343 0.121 Uiso 0.44(2) 1 calc PG A 2 H18D H -0.1582 -0.1104 0.2067 0.121 Uiso 0.44(2) 1 calc PG A 2 C19B C -0.381(4) -0.027(4) 0.238(4) 0.093(9) Uiso 0.44(2) 1 d PG A 2 H19D H -0.3977 -0.1021 0.2286 0.121 Uiso 0.44(2) 1 calc PG A 2 H19E H -0.4587 0.0128 0.2978 0.121 Uiso 0.44(2) 1 calc PG A 2 H19F H -0.3885 0.0405 0.1692 0.121 Uiso 0.44(2) 1 calc PG A 2 C20 C -0.132(2) 0.2797(17) -0.0256(14) 0.086(6) Uani 1 1 d . . . O14 O -0.0927(18) 0.2055(12) -0.0761(9) 0.105(5) Uani 1 1 d . B . C21A C -0.201(6) 0.413(7) -0.076(4) 0.102(9) Uiso 0.60(3) 1 d PG B 1 H21A H -0.1119 0.4392 -0.1103 0.133 Uiso 0.60(3) 1 calc PG B 1 H21B H -0.2599 0.4638 -0.0171 0.133 Uiso 0.60(3) 1 calc PG B 1 C22A C -0.291(5) 0.442(4) -0.153(3) 0.122(12) Uiso 0.60(3) 1 d PG B 1 H22A H -0.3270 0.5375 -0.1853 0.158 Uiso 0.60(3) 1 calc PG B 1 H22B H -0.2310 0.3917 -0.2118 0.158 Uiso 0.60(3) 1 calc PG B 1 H22C H -0.3802 0.4165 -0.1179 0.158 Uiso 0.60(3) 1 calc PG B 1 C21B C -0.225(8) 0.412(11) -0.064(6) 0.102(9) Uiso 0.40(3) 1 d PG B 2 H21C H -0.1608 0.4151 -0.1372 0.133 Uiso 0.40(3) 1 calc PG B 2 H21D H -0.2356 0.4877 -0.0352 0.133 Uiso 0.40(3) 1 calc PG B 2 C22B C -0.367(7) 0.420(6) -0.072(5) 0.122(12) Uiso 0.40(3) 1 d PG B 2 H22D H -0.4169 0.5038 -0.1220 0.158 Uiso 0.40(3) 1 calc PG B 2 H22E H -0.3553 0.3447 -0.1014 0.158 Uiso 0.40(3) 1 calc PG B 2 H22F H -0.4307 0.4179 0.0014 0.158 Uiso 0.40(3) 1 calc PG B 2 Na1 Na 0.0000 0.5000 0.5000 0.067(3) Uani 1 2 d S . . Na2 Na 0.0000 0.0000 0.0000 0.102(4) Uani 1 2 d S . . Na3 Na -0.0363(8) 0.0942(5) 0.3751(4) 0.071(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0616(9) 0.0360(7) 0.0579(8) -0.0224(6) -0.0130(7) -0.0086(6) C1 0.095(15) 0.045(11) 0.077(12) -0.027(9) -0.030(11) 0.004(10) O1 0.115(12) 0.043(8) 0.110(11) -0.013(7) -0.024(9) -0.004(8) C2 0.116(18) 0.043(10) 0.070(12) -0.020(9) -0.016(12) -0.019(10) O2 0.138(14) 0.098(11) 0.076(9) -0.032(8) 0.007(10) -0.035(10) O3 0.061(7) 0.046(6) 0.058(7) -0.019(5) -0.006(6) -0.022(6) O4 0.100(9) 0.052(7) 0.056(7) -0.013(5) -0.026(6) -0.031(6) C3 0.069(12) 0.053(10) 0.051(10) -0.022(8) -0.016(9) -0.009(9) C4 0.077(14) 0.106(15) 0.064(11) -0.033(11) -0.001(10) -0.040(12) C5 0.092(19) 0.14(2) 0.115(19) -0.028(17) -0.012(15) -0.033(17) O5 0.087(9) 0.036(6) 0.075(8) -0.022(5) -0.016(7) -0.012(6) O6 0.105(10) 0.038(6) 0.077(8) -0.024(5) -0.029(7) -0.014(6) C6 0.071(14) 0.063(12) 0.072(12) -0.018(9) -0.026(10) -0.013(10) C7 0.105(17) 0.062(13) 0.137(19) -0.045(13) -0.055(15) -0.005(12) C8 0.17(3) 0.062(16) 0.26(4) 0.02(2) -0.09(3) 0.012(17) C9 0.053(11) 0.038(9) 0.073(11) -0.017(8) -0.010(9) 0.000(8) O7 0.060(8) 0.065(8) 0.120(10) -0.048(7) -0.021(7) -0.010(6) C10 0.049(12) 0.083(13) 0.133(18) -0.046(13) -0.025(12) -0.013(10) C11 0.045(12) 0.112(17) 0.16(2) -0.073(16) -0.009(13) -0.022(11) Ru2 0.184(2) 0.0491(9) 0.0596(10) -0.0051(7) -0.0459(11) -0.0500(11) C12 0.17(3) 0.090(18) 0.107(19) -0.023(15) -0.019(19) -0.073(19) O8 0.18(2) 0.155(19) 0.19(2) -0.110(17) 0.011(17) -0.049(16) C13 0.13(2) 0.063(13) 0.102(16) 0.011(11) -0.057(14) -0.040(13) O9 0.24(2) 0.115(15) 0.176(19) 0.038(13) -0.123(17) -0.095(16) O10 0.22(2) 0.064(9) 0.091(10) -0.016(8) -0.071(12) -0.034(10) O11 0.113(11) 0.065(8) 0.056(7) -0.022(6) -0.006(7) -0.032(7) C14 0.089(16) 0.043(10) 0.089(15) -0.002(10) -0.023(13) -0.030(10) C15 0.17(3) 0.095(18) 0.13(2) -0.052(17) 0.06(2) -0.038(19) C16 0.21(4) 0.25(5) 0.27(5) -0.11(4) 0.04(4) -0.05(4) O12 0.28(2) 0.077(9) 0.054(8) -0.019(7) -0.013(11) -0.104(12) O13 0.105(11) 0.088(9) 0.069(8) -0.034(7) -0.028(7) -0.021(8) C17 0.083(14) 0.070(12) 0.061(12) -0.004(10) -0.016(10) -0.046(10) C20 0.15(2) 0.063(12) 0.068(12) 0.005(10) -0.053(13) -0.051(12) O14 0.196(17) 0.081(9) 0.052(7) 0.001(7) -0.049(9) -0.058(10) Na1 0.070(6) 0.048(5) 0.093(7) -0.040(5) -0.023(5) -0.007(4) Na2 0.192(13) 0.076(7) 0.052(6) -0.018(5) -0.032(7) -0.054(8) Na3 0.119(6) 0.046(3) 0.053(4) -0.015(3) -0.034(4) -0.021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C2 1.82(2) . ? Ru1 C1 1.858(17) . ? Ru1 C9 1.985(17) . ? Ru1 O3 2.086(10) . ? Ru1 O5 2.153(10) . ? Ru1 O6 2.342(12) . ? Ru1 Na1 3.4114(19) . ? Ru1 Na3 3.533(7) . ? C1 O1 1.132(18) . ? C2 O2 1.18(2) . ? O3 C3 1.264(19) . ? O3 Na1 2.568(10) . ? O4 C3 1.285(17) . ? O4 Na3 2.398(11) . ? O4 Na3 2.428(12) 2_556 ? C3 C4 1.52(2) . ? C4 C5 1.50(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? O5 C6 1.27(2) . ? O5 Na1 2.462(11) . ? O6 C6 1.28(2) . ? O6 Na3 2.449(12) . ? C6 C7 1.53(3) . ? C7 C8 1.45(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 O7 1.256(17) . ? C9 C10 1.50(2) . ? O7 Na1 2.313(11) . ? C10 C11 1.53(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? Ru2 C13 1.79(2) . ? Ru2 C12 1.87(3) . ? Ru2 C20 1.975(17) . ? Ru2 O12 2.077(13) . ? Ru2 O10 2.164(17) . ? Ru2 Na2 3.2529(19) . ? Ru2 Na3 3.667(6) . ? C12 O8 1.12(3) . ? C13 O9 1.18(2) . ? O10 C14 1.24(2) . ? O10 Na2 2.449(16) . ? O11 C14 1.25(2) . ? O11 Na3 2.334(14) . ? C14 C15 1.57(3) . ? C15 C16 1.461(19) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? O12 C17 1.214(19) . ? O12 Na2 2.338(15) . ? O13 C17 1.235(19) . ? O13 Na3 2.321(14) . ? C17 C18B 1.58(6) . ? C17 C18A 1.57(4) . ? C18A C19A 1.5129 . ? C18A H18A 1.0800 . ? C18A H18B 1.0800 . ? C19A H19A 1.0800 . ? C19A H19B 1.0800 . ? C19A H19C 1.0800 . ? C18B C19B 1.5130 . ? C18B H18C 1.0801 . ? C18B H18D 1.0800 . ? C19B H19D 1.0800 . ? C19B H19E 1.0801 . ? C19B H19F 1.0800 . ? C20 O14 1.20(2) . ? C20 C21B 1.54(11) . ? C20 C21A 1.54(7) . ? C20 Na2 3.11(2) . ? O14 Na2 2.348(13) . ? C21A C22A 1.5130 . ? C21A H21A 1.0799 . ? C21A H21B 1.0800 . ? C22A H22A 1.0800 . ? C22A H22B 1.0800 . ? C22A H22C 1.0800 . ? C21B C22B 1.5129 . ? C21B H21C 1.0800 . ? C21B H21D 1.0800 . ? C22B H22D 1.0800 . ? C22B H22E 1.0801 . ? C22B H22F 1.0800 . ? Na1 O7 2.313(11) 2_566 ? Na1 O5 2.462(11) 2_566 ? Na1 O3 2.568(10) 2_566 ? Na1 Ru1 3.4114(19) 2_566 ? Na2 O12 2.338(15) 2 ? Na2 O14 2.348(13) 2 ? Na2 O10 2.449(16) 2 ? Na2 C20 3.11(2) 2 ? Na2 Ru2 3.2529(19) 2 ? Na3 O4 2.428(12) 2_556 ? Na3 Na3 3.685(12) 2_556 ? 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 Ru1 C1 87.3(8) . . ? C2 Ru1 C9 90.7(8) . . ? C1 Ru1 C9 91.9(7) . . ? C2 Ru1 O3 176.8(6) . . ? C1 Ru1 O3 95.8(6) . . ? C9 Ru1 O3 90.0(5) . . ? C2 Ru1 O5 96.3(6) . . ? C1 Ru1 O5 170.8(7) . . ? C9 Ru1 O5 96.5(5) . . ? O3 Ru1 O5 80.5(4) . . ? C2 Ru1 O6 97.0(7) . . ? C1 Ru1 O6 113.0(7) . . ? C9 Ru1 O6 154.1(5) . . ? O3 Ru1 O6 81.1(4) . . ? O5 Ru1 O6 58.2(4) . . ? C2 Ru1 Na1 128.9(5) . . ? C1 Ru1 Na1 136.0(5) . . ? C9 Ru1 Na1 67.2(4) . . ? O3 Ru1 Na1 48.7(3) . . ? O5 Ru1 Na1 46.0(3) . . ? O6 Ru1 Na1 89.1(2) . . ? C2 Ru1 Na3 98.2(6) . . ? C1 Ru1 Na3 69.5(6) . . ? C9 Ru1 Na3 158.8(5) . . ? O3 Ru1 Na3 82.2(3) . . ? O5 Ru1 Na3 101.5(4) . . ? O6 Ru1 Na3 43.7(3) . . ? Na1 Ru1 Na3 119.15(12) . . ? O1 C1 Ru1 178.4(17) . . ? O2 C2 Ru1 175.3(19) . . ? C3 O3 Ru1 121.4(9) . . ? C3 O3 Na1 138.9(9) . . ? Ru1 O3 Na1 93.7(4) . . ? C3 O4 Na3 129.5(10) . . ? C3 O4 Na3 130.7(10) . 2_556 ? Na3 O4 Na3 99.5(4) . 2_556 ? O3 C3 O4 124.0(15) . . ? O3 C3 C4 118.5(14) . . ? O4 C3 C4 117.5(17) . . ? C5 C4 C3 111.5(16) . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6 O5 Ru1 95.6(10) . . ? C6 O5 Na1 119.5(11) . . ? Ru1 O5 Na1 95.1(4) . . ? C6 O6 Ru1 86.7(10) . . ? C6 O6 Na3 167.6(12) . . ? Ru1 O6 Na3 95.0(4) . . ? O5 C6 O6 118.9(16) . . ? O5 C6 C7 120.8(17) . . ? O6 C6 C7 120.2(17) . . ? C8 C7 C6 114(2) . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O7 C9 C10 118.9(15) . . ? O7 C9 Ru1 113.8(12) . . ? C10 C9 Ru1 127.3(11) . . ? C9 O7 Na1 125.7(11) . . ? C9 C10 C11 115.8(15) . . ? C9 C10 H10A 108.3 . . ? C11 C10 H10A 108.3 . . ? C9 C10 H10B 108.3 . . ? C11 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 Ru2 C12 90.1(11) . . ? C13 Ru2 C20 92.2(8) . . ? C12 Ru2 C20 89.8(11) . . ? C13 Ru2 O12 175.3(9) . . ? C12 Ru2 O12 93.9(9) . . ? C20 Ru2 O12 90.4(7) . . ? C13 Ru2 O10 92.5(9) . . ? C12 Ru2 O10 175.6(9) . . ? C20 Ru2 O10 93.6(8) . . ? O12 Ru2 O10 83.4(7) . . ? C13 Ru2 Na2 132.2(8) . . ? C12 Ru2 Na2 130.7(8) . . ? C20 Ru2 Na2 67.9(6) . . ? O12 Ru2 Na2 45.8(4) . . ? O10 Ru2 Na2 48.8(4) . . ? C13 Ru2 Na3 96.4(7) . . ? C12 Ru2 Na3 86.5(8) . . ? C20 Ru2 Na3 170.7(6) . . ? O12 Ru2 Na3 81.2(4) . . ? O10 Ru2 Na3 89.7(4) . . ? Na2 Ru2 Na3 108.28(10) . . ? O8 C12 Ru2 179(3) . . ? O9 C13 Ru2 176(2) . . ? C14 O10 Ru2 104.4(13) . . ? C14 O10 Na2 129.0(13) . . ? Ru2 O10 Na2 89.5(7) . . ? C14 O11 Na3 157.7(12) . . ? O10 C14 O11 120.5(19) . . ? O10 C14 C15 125(2) . . ? O11 C14 C15 114.1(19) . . ? C16 C15 C14 112(3) . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 O12 Ru2 116.4(11) . . ? C17 O12 Na2 136.5(13) . . ? Ru2 O12 Na2 94.7(6) . . ? C17 O13 Na3 139.2(13) . . ? O12 C17 O13 122.8(16) . . ? O12 C17 C18B 127(3) . . ? O13 C17 C18B 110(2) . . ? O12 C17 C18A 106.8(18) . . ? O13 C17 C18A 130.1(19) . . ? C18B C17 C18A 23(2) . . ? C19A C18A C17 111(3) . . ? C17 C18A H18A 66.0 . . ? C17 C18A H18B 138.4 . . ? C19B C18B C17 105(4) . . ? C19B C18B H18C 109.8 . . ? C17 C18B H18C 134.3 . . ? C19B C18B H18D 109.8 . . ? C17 C18B H18D 86.6 . . ? H18C C18B H18D 108.2 . . ? C18B C19B H19D 109.5 . . ? C18B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C18B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? O14 C20 C21B 121(3) . . ? O14 C20 C21A 118(2) . . ? C21B C20 C21A 10(5) . . ? O14 C20 Ru2 116.9(14) . . ? C21B C20 Ru2 122(3) . . ? C21A C20 Ru2 125(2) . . ? O14 C20 Na2 41.5(9) . . ? C21B C20 Na2 159(3) . . ? C21A C20 Na2 159(2) . . ? Ru2 C20 Na2 76.0(6) . . ? C20 O14 Na2 118.8(11) . . ? C22A C21A C20 117(5) . . ? C20 C21A H21A 102.8 . . ? C20 C21A H21B 108.3 . . ? C22B C21B C20 110(7) . . ? C22B C21B H21C 109.8 . . ? C20 C21B H21C 92.5 . . ? C22B C21B H21D 109.8 . . ? C20 C21B H21D 124.2 . . ? H21C C21B H21D 108.2 . . ? C21B C22B H22D 109.5 . . ? C21B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C21B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? O7 Na1 O7 180.000(1) 2_566 . ? O7 Na1 O5 100.8(4) 2_566 . ? O7 Na1 O5 79.2(4) . . ? O7 Na1 O5 79.2(4) 2_566 2_566 ? O7 Na1 O5 100.8(4) . 2_566 ? O5 Na1 O5 180.000(1) . 2_566 ? O7 Na1 O3 73.7(4) 2_566 2_566 ? O7 Na1 O3 106.3(4) . 2_566 ? O5 Na1 O3 114.0(3) . 2_566 ? O5 Na1 O3 66.0(3) 2_566 2_566 ? O7 Na1 O3 106.3(4) 2_566 . ? O7 Na1 O3 73.7(4) . . ? O5 Na1 O3 66.0(3) . . ? O5 Na1 O3 114.0(3) 2_566 . ? O3 Na1 O3 180.000(1) 2_566 . ? O7 Na1 Ru1 53.2(3) 2_566 2_566 ? O7 Na1 Ru1 126.8(3) . 2_566 ? O5 Na1 Ru1 141.0(2) . 2_566 ? O5 Na1 Ru1 39.0(2) 2_566 2_566 ? O3 Na1 Ru1 37.6(2) 2_566 2_566 ? O3 Na1 Ru1 142.4(2) . 2_566 ? O7 Na1 Ru1 126.8(3) 2_566 . ? O7 Na1 Ru1 53.2(3) . . ? O5 Na1 Ru1 39.0(2) . . ? O5 Na1 Ru1 141.0(2) 2_566 . ? O3 Na1 Ru1 142.4(2) 2_566 . ? O3 Na1 Ru1 37.6(2) . . ? Ru1 Na1 Ru1 180.00(4) 2_566 . ? O12 Na2 O12 180.0(12) . 2 ? O12 Na2 O14 79.1(5) . . ? O12 Na2 O14 100.9(5) 2 . ? O12 Na2 O14 100.9(5) . 2 ? O12 Na2 O14 79.1(5) 2 2 ? O14 Na2 O14 180.0(12) . 2 ? O12 Na2 O10 72.2(6) . . ? O12 Na2 O10 107.8(6) 2 . ? O14 Na2 O10 77.8(5) . . ? O14 Na2 O10 102.2(5) 2 . ? O12 Na2 O10 107.8(6) . 2 ? O12 Na2 O10 72.2(6) 2 2 ? O14 Na2 O10 102.2(5) . 2 ? O14 Na2 O10 77.8(5) 2 2 ? O10 Na2 O10 180.0(6) . 2 ? O12 Na2 C20 61.9(5) . . ? O12 Na2 C20 118.1(5) 2 . ? O14 Na2 C20 19.7(4) . . ? O14 Na2 C20 160.3(4) 2 . ? O10 Na2 C20 64.6(5) . . ? O10 Na2 C20 115.4(5) 2 . ? O12 Na2 C20 118.1(5) . 2 ? O12 Na2 C20 61.9(5) 2 2 ? O14 Na2 C20 160.3(4) . 2 ? O14 Na2 C20 19.7(4) 2 2 ? O10 Na2 C20 115.4(5) . 2 ? O10 Na2 C20 64.6(5) 2 2 ? C20 Na2 C20 180.0(12) . 2 ? O12 Na2 Ru2 39.5(3) . . ? O12 Na2 Ru2 140.5(3) 2 . ? O14 Na2 Ru2 55.6(3) . . ? O14 Na2 Ru2 124.4(3) 2 . ? O10 Na2 Ru2 41.7(4) . . ? O10 Na2 Ru2 138.3(4) 2 . ? C20 Na2 Ru2 36.1(3) . . ? C20 Na2 Ru2 143.9(3) 2 . ? O12 Na2 Ru2 140.5(3) . 2 ? O12 Na2 Ru2 39.5(3) 2 2 ? O14 Na2 Ru2 124.4(3) . 2 ? O14 Na2 Ru2 55.6(3) 2 2 ? O10 Na2 Ru2 138.3(4) . 2 ? O10 Na2 Ru2 41.7(4) 2 2 ? C20 Na2 Ru2 143.9(3) . 2 ? C20 Na2 Ru2 36.1(3) 2 2 ? Ru2 Na2 Ru2 180.00(10) . 2 ? O13 Na3 O11 85.6(5) . . ? O13 Na3 O4 142.4(5) . . ? O11 Na3 O4 132.0(5) . . ? O13 Na3 O4 91.0(5) . 2_556 ? O11 Na3 O4 106.2(4) . 2_556 ? O4 Na3 O4 80.5(4) . 2_556 ? O13 Na3 O6 107.0(5) . . ? O11 Na3 O6 84.8(4) . . ? O4 Na3 O6 79.6(4) . . ? O4 Na3 O6 159.8(4) 2_556 . ? O13 Na3 Ru1 144.7(4) . . ? O11 Na3 Ru1 77.6(3) . . ? O4 Na3 Ru1 60.9(3) . . ? O4 Na3 Ru1 123.4(3) 2_556 . ? O6 Na3 Ru1 41.3(3) . . ? O13 Na3 Ru2 52.8(3) . . ? O11 Na3 Ru2 45.2(3) . . ? O4 Na3 Ru2 150.8(3) . . ? O4 Na3 Ru2 128.6(3) 2_556 . ? O6 Na3 Ru2 71.2(3) . . ? Ru1 Na3 Ru2 94.76(16) . . ? O13 Na3 Na3 121.8(5) . 2_556 ? O11 Na3 Na3 128.3(5) . 2_556 ? O4 Na3 Na3 40.5(3) . 2_556 ? O4 Na3 Na3 39.9(3) 2_556 2_556 ? O6 Na3 Na3 120.1(4) . 2_556 ? Ru1 Na3 Na3 92.7(2) . 2_556 ? Ru2 Na3 Na3 168.2(3) . 2_556 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.865 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.123 #===END