# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Jingyang Niu' _publ_contact_author_email jyniu@henu.edu.cn _publ_section_title ; Novel Octatungstate-Supported Tricarbonyl Metal Derivatives: {[H2W8O30][M(CO)3]2}8- (M = MnI and ReI) ; _publ_author_name 'Jingyang Niu' # Attachment '- 809237-809239.cif' data_njy1 _database_code_depnum_ccdc_archive 'CCDC 809237' #TrackingRef '- 809237-809239.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H54 Mn2 Na2 O59 W8' _chemical_formula_weight 2697.15 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6124(8) _cell_length_b 12.1841(10) _cell_length_c 14.0241(11) _cell_angle_alpha 71.5230(10) _cell_angle_beta 87.4540(10) _cell_angle_gamma 71.1410(10) _cell_volume 1471.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3996 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.37 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1226 _exptl_absorpt_coefficient_mu 16.117 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.0976 _exptl_absorpt_correction_T_max 0.1595 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7069 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5000 _reflns_number_gt 3641 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1373P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens notdet _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5000 _refine_ls_number_parameters 361 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1016 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.2061 _refine_ls_wR_factor_gt 0.1823 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.064 _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 Na1 Na -1.1813(11) 0.5342(9) 0.5200(8) 0.047(3) Uani 1 1 d . . . Mn1 Mn -0.9267(4) -0.3261(3) 0.8293(2) 0.0298(8) Uani 1 1 d . . . W1 W -0.69813(9) -0.29023(8) 0.66234(6) 0.0252(3) Uani 1 1 d . . . W2 W -0.86086(10) -0.07443(8) 0.77131(6) 0.0234(3) Uani 1 1 d . . . W3 W -1.07262(9) -0.14517(7) 0.62241(6) 0.0187(3) Uani 1 1 d . . . W4 W -1.15000(9) 0.19008(7) 0.60055(6) 0.0206(3) Uani 1 1 d . . . O1 O -0.6128(19) -0.4461(14) 0.7090(12) 0.042(4) Uani 1 1 d . . . O2 O -0.5502(18) -0.2308(16) 0.6502(14) 0.045(4) Uani 1 1 d . . . O3 O -0.7003(18) -0.0360(15) 0.7515(13) 0.043(4) Uani 1 1 d . . . O4 O -0.8869(16) -0.0808(14) 0.8971(12) 0.033(4) Uani 1 1 d U . . O5 O -1.2245(17) -0.1954(13) 0.6447(10) 0.029(4) Uani 1 1 d . . . O6 O -1.118(2) 0.3205(14) 0.6081(12) 0.042(4) Uani 1 1 d . . . O7 O -1.3013(18) 0.1905(16) 0.6738(11) 0.043(5) Uani 1 1 d . . . O8 O -0.7327(16) -0.2672(12) 0.5260(10) 0.026(3) Uani 1 1 d . . . O9 O -0.9124(15) -0.3051(12) 0.6808(10) 0.023(3) Uani 1 1 d . . . O10 O -0.7534(16) -0.2556(13) 0.7942(10) 0.026(3) Uani 1 1 d . . . O11 O -1.0254(16) -0.1567(12) 0.4977(10) 0.022(3) Uani 1 1 d . . . O12 O -1.1584(16) 0.0169(13) 0.5845(10) 0.026(3) Uani 1 1 d . . . O13 O -0.9977(16) 0.0779(12) 0.7043(10) 0.026(3) Uani 1 1 d . . . O14 O -1.0341(14) -0.1459(12) 0.7609(10) 0.019(3) Uani 1 1 d U . . O15 O -0.8567(14) -0.1008(13) 0.6229(10) 0.026(3) Uani 1 1 d . . . O1A O -0.926(3) -0.3317(18) 1.0401(12) 0.067(7) Uani 1 1 d . . . O2A O -0.755(2) -0.5886(16) 0.9027(14) 0.062(6) Uani 1 1 d . . . O3A O -1.197(3) -0.395(2) 0.8645(18) 0.072(6) Uani 1 1 d U . . C1 C -0.928(3) -0.323(2) 0.956(2) 0.042(6) Uani 1 1 d U . . C2 C -0.820(3) -0.484(2) 0.8720(18) 0.059(9) Uani 1 1 d . . . C3 C -1.087(3) -0.369(2) 0.8457(19) 0.044(7) Uani 1 1 d . . . O1W O 0.1682(18) -0.3422(13) 0.2173(10) 0.033(4) Uani 1 1 d . . . O2W O 0.3801(17) -0.1455(14) 0.1607(11) 0.035(4) Uani 1 1 d . . . O3W O -0.5394(16) 0.0988(15) 0.3062(16) 0.053(6) Uani 1 1 d . . . O4W O -0.957(2) 0.5204(17) 0.6094(14) 0.051(5) Uani 1 1 d . . . O5W O -1.274(2) 0.5590(18) 0.6761(16) 0.064(6) Uani 1 1 d . . . O6W O -1.221(2) 0.748(2) 0.4239(17) 0.075(7) Uani 1 1 d . . . O7W O -1.422(3) 0.577(2) 0.439(2) 0.084(8) Uani 1 1 d . . . O8W O -0.139(3) 0.1329(19) -0.1045(15) 0.075(7) Uani 1 1 d . . . O9W O -0.089(3) -0.292(2) 0.2333(16) 0.089(8) Uani 1 1 d . . . O10W O 0.309(3) 0.059(2) 0.175(2) 0.099(9) Uani 1 1 d . . . O11W O -0.452(3) 0.364(3) 0.043(2) 0.035(7) Uani 0.50 1 d PU . . O12W O -0.514(3) -0.092(3) 0.433(2) 0.035(7) Uani 0.50 1 d PU . . O13W O -0.601(3) 0.643(3) 0.155(2) 0.035(7) Uani 0.50 1 d PU . . 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 Na1 0.057(7) 0.038(6) 0.045(6) -0.010(5) 0.014(5) -0.021(5) Mn1 0.050(2) 0.0200(17) 0.0094(16) 0.0057(13) 0.0020(14) -0.0088(15) W1 0.0298(5) 0.0243(5) 0.0111(4) -0.0016(3) -0.0017(3) 0.0011(4) W2 0.0338(5) 0.0209(5) 0.0086(4) -0.0003(3) -0.0014(3) -0.0037(4) W3 0.0257(5) 0.0182(5) 0.0066(4) 0.0018(3) 0.0042(3) -0.0060(3) W4 0.0302(5) 0.0177(5) 0.0075(4) -0.0009(3) 0.0038(3) -0.0029(3) O1 0.056(11) 0.026(9) 0.021(8) -0.001(7) -0.003(8) 0.011(8) O2 0.038(10) 0.044(11) 0.061(12) -0.034(9) 0.011(9) -0.008(8) O3 0.037(10) 0.041(10) 0.041(10) -0.004(8) 0.000(8) -0.006(8) O4 0.033(4) 0.033(4) 0.032(4) -0.0106(15) 0.0021(10) -0.0102(15) O5 0.046(9) 0.022(8) 0.013(7) 0.004(6) 0.008(6) -0.014(7) O6 0.072(13) 0.018(8) 0.032(10) -0.008(7) 0.006(8) -0.011(8) O7 0.044(10) 0.053(11) 0.010(8) 0.002(7) 0.010(7) -0.002(8) O8 0.045(9) 0.023(8) 0.011(7) -0.006(6) 0.001(6) -0.011(7) O9 0.031(8) 0.020(7) 0.017(7) 0.003(6) -0.004(6) -0.013(6) O10 0.043(9) 0.027(8) 0.010(7) -0.007(6) -0.001(6) -0.012(7) O11 0.034(8) 0.015(7) 0.013(7) 0.000(5) 0.007(6) -0.005(6) O12 0.032(8) 0.036(9) 0.019(8) -0.009(7) 0.001(6) -0.021(7) O13 0.042(9) 0.019(8) 0.006(7) 0.004(6) 0.004(6) -0.004(6) O14 0.019(3) 0.019(3) 0.018(3) -0.0056(13) 0.0015(10) -0.0058(13) O15 0.017(7) 0.037(9) 0.019(8) -0.005(7) 0.011(6) -0.007(6) O1A 0.14(2) 0.057(13) 0.012(9) -0.004(8) 0.000(11) -0.049(13) O2A 0.104(17) 0.024(10) 0.037(11) 0.008(8) 0.001(11) -0.011(10) O3A 0.072(6) 0.073(6) 0.072(6) -0.023(2) 0.0048(11) -0.024(2) C1 0.043(6) 0.042(6) 0.042(6) -0.013(2) 0.0028(11) -0.014(2) C2 0.09(2) 0.033(16) 0.019(13) 0.002(11) 0.013(13) 0.020(14) C3 0.065(18) 0.041(15) 0.025(13) -0.008(11) -0.004(12) -0.017(13) O1W 0.059(11) 0.029(9) 0.006(7) -0.005(6) 0.006(7) -0.010(7) O2W 0.043(10) 0.040(10) 0.020(8) -0.014(7) 0.000(7) -0.007(7) O3W 0.020(9) 0.034(10) 0.106(17) -0.031(11) 0.037(10) -0.007(7) O4W 0.062(12) 0.049(12) 0.043(11) -0.020(9) 0.022(9) -0.018(9) O5W 0.064(14) 0.059(13) 0.058(14) -0.015(11) 0.001(11) -0.008(10) O6W 0.067(15) 0.080(16) 0.065(15) 0.009(12) -0.018(12) -0.036(12) O7W 0.086(17) 0.11(2) 0.084(18) -0.050(16) -0.012(14) -0.050(15) O8W 0.106(19) 0.064(15) 0.038(12) -0.021(11) -0.022(12) 0.006(13) O9W 0.11(2) 0.092(18) 0.035(12) 0.007(12) -0.004(12) -0.014(15) O10W 0.065(15) 0.11(2) 0.16(3) -0.08(2) 0.053(17) -0.056(15) O11W 0.035(7) 0.035(7) 0.035(7) -0.011(3) 0.0020(11) -0.011(3) O12W 0.035(7) 0.035(7) 0.035(7) -0.011(3) 0.0024(11) -0.012(3) O13W 0.035(7) 0.035(7) 0.034(7) -0.011(3) 0.0022(11) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na1 O4W 2.34(2) 2_366 ? Na1 O6 2.383(18) . ? Na1 O5W 2.40(2) . ? Na1 O6W 2.43(2) . ? Na1 O7W 2.45(2) . ? Na1 O4W 2.47(2) . ? Na1 Na1 3.38(2) 2_366 ? Mn1 C3 1.77(3) . ? Mn1 C2 1.78(2) . ? Mn1 C1 1.79(3) . ? Mn1 O9 2.020(14) . ? Mn1 O14 2.023(13) . ? Mn1 O10 2.082(15) . ? Mn1 W3 3.091(3) . ? Mn1 W1 3.164(4) . ? Mn1 W2 3.177(3) . ? W1 O1 1.721(15) . ? W1 O2 1.773(18) . ? W1 O8 1.871(13) . ? W1 O10 2.036(14) . ? W1 O9 2.123(14) . ? W1 O15 2.224(14) . ? W2 O3 1.739(17) . ? W2 O4 1.752(16) . ? W2 O13 1.867(13) . ? W2 O10 2.037(14) . ? W2 O14 2.144(13) . ? W2 O15 2.200(15) . ? W3 O5 1.738(15) . ? W3 O12 1.784(15) . ? W3 O11 1.824(13) . ? W3 O14 1.989(13) . ? W3 O9 2.000(13) . ? W3 O15 2.309(14) . ? W4 O7 1.742(16) . ? W4 O6 1.747(16) . ? W4 O8 1.934(13) 2_356 ? W4 O13 1.940(13) . ? W4 O11 2.148(14) 2_356 ? W4 O12 2.219(14) . ? O8 W4 1.934(13) 2_356 ? O11 W4 2.148(13) 2_356 ? O1A C1 1.15(3) . ? O2A C2 1.17(3) . ? O3A C3 1.19(3) . ? O4W Na1 2.34(2) 2_366 ? 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 O4W Na1 O6 86.8(7) 2_366 . ? O4W Na1 O5W 167.0(8) 2_366 . ? O6 Na1 O5W 84.9(7) . . ? O4W Na1 O6W 88.5(8) 2_366 . ? O6 Na1 O6W 174.2(8) . . ? O5W Na1 O6W 99.1(9) . . ? O4W Na1 O7W 95.8(9) 2_366 . ? O6 Na1 O7W 101.3(8) . . ? O5W Na1 O7W 95.7(9) . . ? O6W Na1 O7W 82.6(8) . . ? O4W Na1 O4W 91.0(7) 2_366 . ? O6 Na1 O4W 85.1(7) . . ? O5W Na1 O4W 78.4(7) . . ? O6W Na1 O4W 91.5(7) . . ? O7W Na1 O4W 170.9(9) . . ? O4W Na1 Na1 47.0(6) 2_366 2_366 ? O6 Na1 Na1 84.2(6) . 2_366 ? O5W Na1 Na1 121.9(7) . 2_366 ? O6W Na1 Na1 90.1(7) . 2_366 ? O7W Na1 Na1 142.5(9) . 2_366 ? O4W Na1 Na1 43.9(5) . 2_366 ? C3 Mn1 C2 88.3(14) . . ? C3 Mn1 C1 90.4(12) . . ? C2 Mn1 C1 90.1(12) . . ? C3 Mn1 O9 97.5(9) . . ? C2 Mn1 O9 95.9(9) . . ? C1 Mn1 O9 170.1(9) . . ? C3 Mn1 O14 95.1(9) . . ? C2 Mn1 O14 171.5(9) . . ? C1 Mn1 O14 97.6(9) . . ? O9 Mn1 O14 76.0(6) . . ? C3 Mn1 O10 172.4(9) . . ? C2 Mn1 O10 98.1(12) . . ? C1 Mn1 O10 93.6(9) . . ? O9 Mn1 O10 77.9(5) . . ? O14 Mn1 O10 78.0(5) . . ? C3 Mn1 W3 86.8(8) . . ? C2 Mn1 W3 133.6(9) . . ? C1 Mn1 W3 135.9(8) . . ? O9 Mn1 W3 39.5(4) . . ? O14 Mn1 W3 39.2(4) . . ? O10 Mn1 W3 85.9(4) . . ? C3 Mn1 W1 137.8(8) . . ? C2 Mn1 W1 87.6(9) . . ? C1 Mn1 W1 131.5(8) . . ? O9 Mn1 W1 41.4(4) . . ? O14 Mn1 W1 84.6(4) . . ? O10 Mn1 W1 39.3(4) . . ? W3 Mn1 W1 66.72(6) . . ? C3 Mn1 W2 135.2(9) . . ? C2 Mn1 W2 136.2(12) . . ? C1 Mn1 W2 85.6(8) . . ? O9 Mn1 W2 84.7(4) . . ? O14 Mn1 W2 41.8(4) . . ? O10 Mn1 W2 39.0(4) . . ? W3 Mn1 W2 66.78(6) . . ? W1 Mn1 W2 64.26(7) . . ? O1 W1 O2 103.5(8) . . ? O1 W1 O8 101.6(7) . . ? O2 W1 O8 98.1(8) . . ? O1 W1 O10 99.2(7) . . ? O2 W1 O10 92.7(7) . . ? O8 W1 O10 153.5(6) . . ? O1 W1 O9 93.2(7) . . ? O2 W1 O9 161.5(7) . . ? O8 W1 O9 86.0(6) . . ? O10 W1 O9 76.6(6) . . ? O1 W1 O15 165.2(7) . . ? O2 W1 O15 89.6(7) . . ? O8 W1 O15 82.9(6) . . ? O10 W1 O15 73.0(5) . . ? O9 W1 O15 73.0(5) . . ? O1 W1 Mn1 86.7(6) . . ? O2 W1 Mn1 133.0(6) . . ? O8 W1 Mn1 125.0(5) . . ? O10 W1 Mn1 40.3(4) . . ? O9 W1 Mn1 39.0(4) . . ? O15 W1 Mn1 79.3(3) . . ? O3 W2 O4 101.3(8) . . ? O3 W2 O13 99.3(7) . . ? O4 W2 O13 101.0(7) . . ? O3 W2 O10 93.6(7) . . ? O4 W2 O10 98.6(6) . . ? O13 W2 O10 153.9(6) . . ? O3 W2 O14 162.6(7) . . ? O4 W2 O14 94.2(6) . . ? O13 W2 O14 85.2(6) . . ? O10 W2 O14 76.3(5) . . ? O3 W2 O15 91.3(7) . . ? O4 W2 O15 165.6(6) . . ? O13 W2 O15 83.6(6) . . ? O10 W2 O15 73.5(5) . . ? O14 W2 O15 72.5(5) . . ? O3 W2 Mn1 133.6(5) . . ? O4 W2 Mn1 86.9(5) . . ? O13 W2 Mn1 124.1(5) . . ? O10 W2 Mn1 40.1(4) . . ? O14 W2 Mn1 38.9(3) . . ? O15 W2 Mn1 79.3(4) . . ? O5 W3 O12 101.5(6) . . ? O5 W3 O11 102.8(7) . . ? O12 W3 O11 97.3(6) . . ? O5 W3 O14 98.2(6) . . ? O12 W3 O14 89.7(6) . . ? O11 W3 O14 156.0(6) . . ? O5 W3 O9 99.4(6) . . ? O12 W3 O9 156.7(6) . . ? O11 W3 O9 88.0(6) . . ? O14 W3 O9 77.2(6) . . ? O5 W3 O15 169.4(6) . . ? O12 W3 O15 84.5(6) . . ? O11 W3 O15 84.9(6) . . ? O14 W3 O15 72.9(5) . . ? O9 W3 O15 73.4(5) . . ? O5 W3 Mn1 89.8(4) . . ? O12 W3 Mn1 129.7(4) . . ? O11 W3 Mn1 128.0(4) . . ? O14 W3 Mn1 40.0(4) . . ? O9 W3 Mn1 40.0(4) . . ? O15 W3 Mn1 79.8(3) . . ? O7 W4 O6 100.4(8) . . ? O7 W4 O8 94.4(7) . 2_356 ? O6 W4 O8 97.1(7) . 2_356 ? O7 W4 O13 97.9(7) . . ? O6 W4 O13 94.0(7) . . ? O8 W4 O13 161.6(6) 2_356 . ? O7 W4 O11 166.9(7) . 2_356 ? O6 W4 O11 92.6(7) . 2_356 ? O8 W4 O11 82.0(6) 2_356 2_356 ? O13 W4 O11 83.0(5) . 2_356 ? O7 W4 O12 87.2(7) . . ? O6 W4 O12 172.0(7) . . ? O8 W4 O12 84.8(6) 2_356 . ? O13 W4 O12 82.2(6) . . ? O11 W4 O12 80.0(5) 2_356 . ? W4 O6 Na1 140.5(10) . . ? W1 O8 W4 153.0(9) . 2_356 ? W3 O9 Mn1 100.5(7) . . ? W3 O9 W1 113.1(6) . . ? Mn1 O9 W1 99.6(6) . . ? W1 O10 W2 111.8(6) . . ? W1 O10 Mn1 100.4(6) . . ? W2 O10 Mn1 100.9(6) . . ? W3 O11 W4 145.4(8) . 2_356 ? W3 O12 W4 145.1(7) . . ? W2 O13 W4 154.0(9) . . ? W3 O14 Mn1 100.8(6) . . ? W3 O14 W2 113.1(6) . . ? Mn1 O14 W2 99.3(5) . . ? W2 O15 W1 99.3(5) . . ? W2 O15 W3 99.8(5) . . ? W1 O15 W3 98.7(6) . . ? O1A C1 Mn1 174(2) . . ? O2A C2 Mn1 178(3) . . ? O3A C3 Mn1 174(2) . . ? Na1 O4W Na1 89.0(7) 2_366 . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 4.067 _refine_diff_density_min -5.131 _refine_diff_density_rms 0.573 data_njy3 _database_code_depnum_ccdc_archive 'CCDC 809238' #TrackingRef '- 809237-809239.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H50 Mn3 Na6 O60 W8' _chemical_formula_weight 2856.00 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.118(4) _cell_length_b 11.519(4) _cell_length_c 12.269(4) _cell_angle_alpha 98.291(5) _cell_angle_beta 103.668(5) _cell_angle_gamma 105.798(5) _cell_volume 1432.0(8) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4461 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.43 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1297 _exptl_absorpt_coefficient_mu 16.802 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1131 _exptl_absorpt_correction_T_max 0.2020 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7288 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4993 _reflns_number_gt 4492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+5.3625P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens notdet _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4993 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 W1 W 0.66029(3) 0.76603(3) 0.95254(3) 0.01451(11) Uani 1 1 d . . . W2 W 0.67497(3) 0.97576(3) 0.78536(3) 0.01380(11) Uani 1 1 d . . . W3 W 0.91765(3) 0.84197(3) 0.83928(3) 0.01199(11) Uani 1 1 d . . . W4 W 0.98626(3) 0.81590(3) 1.15441(3) 0.01305(11) Uani 1 1 d . . . Mn1 Mn 0.63707(14) 0.69729(13) 0.68787(12) 0.0190(3) Uani 1 1 d . . . Mn2 Mn 0.5000 1.0000 1.0000 0.0214(5) Uani 1 2 d S . . Na1 Na 1.0838(5) 0.8923(4) 1.5022(4) 0.0368(11) Uani 1 1 d . . . Na2 Na 0.7717(5) 1.3104(4) 0.8660(5) 0.0426(12) Uani 1 1 d . . . Na3 Na 0.9980(7) 1.5109(5) 0.7874(5) 0.0666(17) Uani 1 1 d . . . O1 O 0.5564(7) 0.6174(6) 0.9349(6) 0.0265(16) Uani 1 1 d . . . O2 O 0.5733(6) 0.9723(6) 0.6526(6) 0.0228(15) Uani 1 1 d . . . O3 O 0.9734(6) 0.7517(6) 0.7513(6) 0.0196(14) Uani 1 1 d . . . O4 O 0.9715(7) 0.8255(6) 1.2919(6) 0.0244(15) Uani 1 1 d . . . O5 O 1.0150(6) 1.0008(6) 0.8436(5) 0.0158(13) Uani 1 1 d . . . O6 O 0.9927(6) 0.6647(6) 1.1218(6) 0.0205(15) Uani 1 1 d . . . O7 O 0.5882(7) 0.8594(7) 1.0248(6) 0.0263(16) Uani 1 1 d . . . O8 O 0.6111(7) 1.0492(6) 0.8831(6) 0.0234(15) Uani 1 1 d . . . O9 O 1.0002(6) 0.8325(6) 0.9825(5) 0.0134(13) Uani 1 1 d . . . O10 O 1.1757(6) 0.8909(6) 1.1989(5) 0.0160(13) Uani 1 1 d . . . O11 O 0.7996(6) 0.7718(6) 1.0761(5) 0.0161(13) Uani 1 1 d . . . O12 O 0.5808(6) 0.8066(6) 0.8016(5) 0.0180(14) Uani 1 1 d . . . O13 O 0.7732(6) 0.8650(6) 0.7196(5) 0.0147(13) Uani 1 1 d . . . O14 O 0.7598(6) 0.7088(6) 0.8435(5) 0.0143(13) Uani 1 1 d . . . O15 O 0.8035(6) 0.9335(6) 0.9349(5) 0.0156(13) Uani 1 1 d . . . O16 O 0.4364(9) 0.4651(8) 0.6742(8) 0.058(3) Uani 1 1 d . . . O17 O 0.4753(10) 0.7167(10) 0.4697(8) 0.059(3) Uani 1 1 d . . . O18 O 0.7497(10) 0.5484(9) 0.5549(8) 0.052(2) Uani 1 1 d . . . C1 C 0.7088(10) 0.6111(10) 0.6074(9) 0.027(2) Uani 1 1 d . . . C2 C 0.5390(12) 0.7116(11) 0.5575(12) 0.040(3) Uani 1 1 d . . . C3 C 0.5148(12) 0.5561(11) 0.6810(9) 0.035(3) Uani 1 1 d . . . O1W O 0.3448(8) 0.8614(8) 0.8486(7) 0.041(2) Uani 1 1 d . . . O2W O 1.1259(8) 1.1020(8) 1.4729(7) 0.0377(19) Uani 1 1 d . . . O3W O 1.3008(9) 0.9027(9) 1.4927(8) 0.046(2) Uani 1 1 d . . . O4W O 1.1950(7) 0.9728(7) 1.7114(7) 0.0347(18) Uani 1 1 d . . . O5W O 1.0462(9) 0.6929(8) 1.5494(8) 0.049(2) Uani 1 1 d . . . O6W O 0.5621(10) 1.3157(11) 0.8620(9) 0.065(3) Uani 1 1 d . . . O7W O 0.8304(10) 1.3239(11) 1.0671(9) 0.065(3) Uani 1 1 d . . . O8W O 0.8552(8) 1.5270(7) 0.8984(7) 0.039(2) Uani 1 1 d . . . O9W O 0.7949(10) 1.3351(9) 0.6753(8) 0.056(3) Uani 1 1 d . . . O10W O 1.1155(10) 1.4876(10) 0.6536(8) 0.063(3) Uani 1 1 d . . . O11W O 1.3030(10) 1.2098(10) 1.6905(9) 0.066(3) Uani 1 1 d . . . O12W O 0.2915(10) 0.4702(11) 0.8566(10) 0.069(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01147(19) 0.0198(2) 0.0144(2) 0.00609(16) 0.00668(15) 0.00474(15) W2 0.01196(19) 0.0184(2) 0.0131(2) 0.00477(15) 0.00547(15) 0.00586(15) W3 0.0128(2) 0.01485(19) 0.00977(19) 0.00141(14) 0.00611(14) 0.00486(15) W4 0.0138(2) 0.0156(2) 0.0119(2) 0.00417(15) 0.00624(15) 0.00534(15) Mn1 0.0195(7) 0.0190(7) 0.0145(7) -0.0002(6) 0.0031(6) 0.0034(6) Mn2 0.0186(11) 0.0301(12) 0.0220(11) 0.0066(9) 0.0117(9) 0.0127(9) Na1 0.041(3) 0.042(3) 0.033(2) 0.010(2) 0.018(2) 0.015(2) Na2 0.038(3) 0.037(3) 0.051(3) 0.000(2) 0.017(2) 0.012(2) Na3 0.099(5) 0.054(3) 0.051(4) 0.013(3) 0.045(3) 0.011(3) O1 0.026(4) 0.029(4) 0.020(4) 0.011(3) 0.006(3) -0.002(3) O2 0.021(4) 0.026(4) 0.020(4) 0.006(3) 0.003(3) 0.008(3) O3 0.022(4) 0.022(3) 0.016(3) 0.000(3) 0.008(3) 0.010(3) O4 0.025(4) 0.030(4) 0.022(4) 0.014(3) 0.009(3) 0.008(3) O5 0.015(3) 0.018(3) 0.014(3) 0.004(3) 0.005(3) 0.004(3) O6 0.021(3) 0.013(3) 0.022(4) 0.000(3) 0.001(3) 0.004(3) O7 0.027(4) 0.039(4) 0.022(4) 0.006(3) 0.013(3) 0.020(3) O8 0.028(4) 0.029(4) 0.026(4) 0.011(3) 0.017(3) 0.017(3) O9 0.016(3) 0.018(3) 0.011(3) 0.008(3) 0.007(3) 0.008(3) O10 0.015(3) 0.015(3) 0.017(3) 0.002(3) 0.003(3) 0.005(3) O11 0.015(3) 0.018(3) 0.014(3) 0.002(3) 0.004(3) 0.003(3) O12 0.022(3) 0.018(3) 0.015(3) 0.009(3) 0.007(3) 0.005(3) O13 0.012(3) 0.017(3) 0.014(3) -0.001(3) 0.005(3) 0.002(3) O14 0.014(3) 0.020(3) 0.007(3) 0.002(3) -0.001(2) 0.006(3) O15 0.014(3) 0.021(3) 0.017(3) 0.005(3) 0.010(3) 0.008(3) O16 0.056(6) 0.042(5) 0.052(6) 0.002(5) 0.022(5) -0.024(5) O17 0.066(7) 0.072(7) 0.026(5) -0.007(5) -0.016(5) 0.033(6) O18 0.060(6) 0.051(6) 0.041(5) -0.008(5) 0.011(5) 0.021(5) C1 0.028(6) 0.027(6) 0.025(6) 0.007(5) 0.007(5) 0.007(5) C2 0.032(7) 0.030(6) 0.046(8) -0.003(6) 0.009(6) 0.001(5) C3 0.042(7) 0.042(7) 0.016(6) 0.000(5) 0.007(5) 0.009(6) O1W 0.037(5) 0.037(5) 0.034(5) 0.008(4) 0.006(4) -0.006(4) O2W 0.039(5) 0.049(5) 0.030(4) 0.015(4) 0.016(4) 0.014(4) O3W 0.047(5) 0.061(6) 0.047(5) 0.031(5) 0.029(5) 0.021(5) O4W 0.030(4) 0.036(4) 0.033(4) 0.003(4) 0.008(4) 0.007(4) O5W 0.067(6) 0.047(5) 0.039(5) 0.009(4) 0.028(5) 0.020(5) O6W 0.046(6) 0.100(8) 0.062(7) 0.040(6) 0.021(5) 0.026(6) O7W 0.051(6) 0.083(7) 0.061(7) 0.044(6) 0.009(5) 0.012(5) O8W 0.049(5) 0.029(4) 0.043(5) 0.005(4) 0.011(4) 0.021(4) O9W 0.063(6) 0.052(6) 0.046(6) 0.002(5) -0.006(5) 0.027(5) O10W 0.063(7) 0.081(7) 0.048(6) 0.000(5) 0.035(5) 0.020(6) O11W 0.061(7) 0.071(7) 0.051(6) 0.002(6) 0.009(5) 0.008(6) O12W 0.047(6) 0.084(8) 0.072(7) 0.044(6) 0.011(5) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.735(7) . ? W1 O7 1.765(7) . ? W1 O11 1.873(6) . ? W1 O12 2.033(6) . ? W1 O14 2.072(6) . ? W1 O15 2.217(6) . ? W1 Mn1 3.1605(18) . ? W2 O2 1.738(7) . ? W2 O8 1.758(6) . ? W2 O10 1.878(6) 2_777 ? W2 O12 2.008(6) . ? W2 O13 2.085(6) . ? W2 O15 2.245(6) . ? W2 Mn1 3.1330(18) . ? W2 Na2 3.624(5) . ? W3 O3 1.724(6) . ? W3 O9 1.814(6) . ? W3 O5 1.841(6) . ? W3 O14 2.009(6) . ? W3 O13 2.009(6) . ? W3 O15 2.275(6) . ? W3 Mn1 3.0817(17) . ? W4 O4 1.724(7) . ? W4 O6 1.754(6) . ? W4 O10 1.952(6) . ? W4 O11 1.957(6) . ? W4 O5 2.112(6) 2_777 ? W4 O9 2.183(6) . ? W4 Na2 3.430(5) 2_777 ? Mn1 C1 1.765(11) . ? Mn1 C2 1.768(14) . ? Mn1 C3 1.790(13) . ? Mn1 O13 2.022(6) . ? Mn1 O14 2.030(6) . ? Mn1 O12 2.063(7) . ? Mn2 O7 2.131(7) 2_677 ? Mn2 O7 2.131(7) . ? Mn2 O8 2.144(7) . ? Mn2 O8 2.144(7) 2_677 ? Mn2 O1W 2.260(8) . ? Mn2 O1W 2.260(8) 2_677 ? Na1 O5W 2.401(10) . ? Na1 O3W 2.414(10) . ? Na1 O2W 2.427(10) . ? Na1 O2W 2.439(9) 2_778 ? Na1 O4W 2.482(9) . ? Na1 O4 2.488(8) . ? Na1 Na1 3.484(9) 2_778 ? Na2 O6W 2.337(11) . ? Na2 O8W 2.350(9) . ? Na2 O7W 2.368(11) . ? Na2 O9W 2.463(12) . ? Na2 O6 2.523(8) 2_777 ? Na2 O10 2.603(8) 2_777 ? Na2 Na3 3.350(8) . ? Na2 W4 3.430(5) 2_777 ? Na3 O8W 2.350(11) . ? Na3 O10W 2.356(11) . ? Na3 O7W 2.425(13) 2_787 ? Na3 O6 2.460(9) 2_777 ? Na3 O9W 2.516(12) . ? Na3 O3 2.945(9) 1_565 ? O3 Na3 2.945(9) 1_545 ? O5 W4 2.112(6) 2_777 ? O6 Na3 2.460(9) 2_777 ? O6 Na2 2.523(8) 2_777 ? O10 W2 1.878(6) 2_777 ? O10 Na2 2.603(8) 2_777 ? O16 C3 1.143(14) . ? O17 C2 1.160(15) . ? O18 C1 1.153(13) . ? O2W Na1 2.439(9) 2_778 ? O7W Na3 2.425(13) 2_787 ? 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 O1 W1 O7 103.0(4) . . ? O1 W1 O11 101.0(3) . . ? O7 W1 O11 99.5(3) . . ? O1 W1 O12 100.4(3) . . ? O7 W1 O12 90.1(3) . . ? O11 W1 O12 153.9(3) . . ? O1 W1 O14 93.4(3) . . ? O7 W1 O14 160.3(3) . . ? O11 W1 O14 87.8(3) . . ? O12 W1 O14 76.1(2) . . ? O1 W1 O15 165.1(3) . . ? O7 W1 O15 90.4(3) . . ? O11 W1 O15 82.9(3) . . ? O12 W1 O15 72.7(2) . . ? O14 W1 O15 72.3(2) . . ? O1 W1 Mn1 87.3(2) . . ? O7 W1 Mn1 129.9(2) . . ? O11 W1 Mn1 126.9(2) . . ? O12 W1 Mn1 39.86(18) . . ? O14 W1 Mn1 39.13(16) . . ? O15 W1 Mn1 79.05(16) . . ? O2 W2 O8 102.8(3) . . ? O2 W2 O10 102.5(3) . 2_777 ? O8 W2 O10 98.0(3) . 2_777 ? O2 W2 O12 97.9(3) . . ? O8 W2 O12 92.6(3) . . ? O10 W2 O12 154.2(3) 2_777 . ? O2 W2 O13 95.5(3) . . ? O8 W2 O13 159.9(3) . . ? O10 W2 O13 85.6(3) 2_777 . ? O12 W2 O13 76.8(3) . . ? O2 W2 O15 165.8(3) . . ? O8 W2 O15 88.3(3) . . ? O10 W2 O15 84.2(2) 2_777 . ? O12 W2 O15 72.5(2) . . ? O13 W2 O15 72.3(2) . . ? O2 W2 Mn1 86.7(2) . . ? O8 W2 Mn1 132.9(2) . . ? O10 W2 Mn1 125.18(19) 2_777 . ? O12 W2 Mn1 40.34(19) . . ? O13 W2 Mn1 39.54(17) . . ? O15 W2 Mn1 79.29(16) . . ? O2 W2 Na2 91.8(2) . . ? O8 W2 Na2 59.3(2) . . ? O10 W2 Na2 43.4(2) 2_777 . ? O12 W2 Na2 151.7(2) . . ? O13 W2 Na2 128.78(18) . . ? O15 W2 Na2 101.57(18) . . ? Mn1 W2 Na2 167.72(8) . . ? O3 W3 O9 103.2(3) . . ? O3 W3 O5 103.3(3) . . ? O9 W3 O5 98.0(3) . . ? O3 W3 O14 97.9(3) . . ? O9 W3 O14 88.7(3) . . ? O5 W3 O14 155.7(3) . . ? O3 W3 O13 99.3(3) . . ? O9 W3 O13 155.0(3) . . ? O5 W3 O13 87.3(3) . . ? O14 W3 O13 77.5(2) . . ? O3 W3 O15 168.4(3) . . ? O9 W3 O15 83.0(2) . . ? O5 W3 O15 85.4(3) . . ? O14 W3 O15 72.2(2) . . ? O13 W3 O15 73.0(2) . . ? O3 W3 Mn1 88.5(2) . . ? O9 W3 Mn1 129.2(2) . . ? O5 W3 Mn1 127.60(19) . . ? O14 W3 Mn1 40.54(17) . . ? O13 W3 Mn1 40.29(18) . . ? O15 W3 Mn1 80.01(16) . . ? O4 W4 O6 100.9(3) . . ? O4 W4 O10 96.7(3) . . ? O6 W4 O10 93.6(3) . . ? O4 W4 O11 96.2(3) . . ? O6 W4 O11 95.1(3) . . ? O10 W4 O11 162.8(3) . . ? O4 W4 O5 92.1(3) . 2_777 ? O6 W4 O5 167.0(3) . 2_777 ? O10 W4 O5 84.2(2) . 2_777 ? O11 W4 O5 84.1(2) . 2_777 ? O4 W4 O9 170.9(3) . . ? O6 W4 O9 88.2(3) . . ? O10 W4 O9 83.6(2) . . ? O11 W4 O9 81.8(2) . . ? O5 W4 O9 78.8(2) 2_777 . ? O4 W4 Na2 108.7(2) . 2_777 ? O6 W4 Na2 45.2(2) . 2_777 ? O10 W4 Na2 48.9(2) . 2_777 ? O11 W4 Na2 135.5(2) . 2_777 ? O5 W4 Na2 129.44(19) 2_777 2_777 ? O9 W4 Na2 78.40(18) . 2_777 ? C1 Mn1 C2 89.0(5) . . ? C1 Mn1 C3 89.0(5) . . ? C2 Mn1 C3 89.7(5) . . ? C1 Mn1 O13 98.0(4) . . ? C2 Mn1 O13 95.5(4) . . ? C3 Mn1 O13 171.4(4) . . ? C1 Mn1 O14 95.4(4) . . ? C2 Mn1 O14 171.5(4) . . ? C3 Mn1 O14 97.7(4) . . ? O13 Mn1 O14 76.7(3) . . ? C1 Mn1 O12 171.0(4) . . ? C2 Mn1 O12 98.8(4) . . ? C3 Mn1 O12 95.4(4) . . ? O13 Mn1 O12 77.0(3) . . ? O14 Mn1 O12 76.3(2) . . ? C1 Mn1 W3 86.2(4) . . ? C2 Mn1 W3 133.4(4) . . ? C3 Mn1 W3 136.4(4) . . ? O13 Mn1 W3 39.98(18) . . ? O14 Mn1 W3 40.01(18) . . ? O12 Mn1 W3 85.26(19) . . ? C1 Mn1 W2 138.0(4) . . ? C2 Mn1 W2 87.2(4) . . ? C3 Mn1 W2 132.7(4) . . ? O13 Mn1 W2 41.04(17) . . ? O14 Mn1 W2 84.63(18) . . ? O12 Mn1 W2 39.05(17) . . ? W3 Mn1 W2 67.13(3) . . ? C1 Mn1 W1 133.8(3) . . ? C2 Mn1 W1 137.0(4) . . ? C3 Mn1 W1 86.8(4) . . ? O13 Mn1 W1 84.72(18) . . ? O14 Mn1 W1 40.08(17) . . ? O12 Mn1 W1 39.15(17) . . ? W3 Mn1 W1 66.60(3) . . ? W2 Mn1 W1 65.02(3) . . ? O7 Mn2 O7 180.000(4) 2_677 . ? O7 Mn2 O8 91.7(3) 2_677 . ? O7 Mn2 O8 88.3(3) . . ? O7 Mn2 O8 88.3(3) 2_677 2_677 ? O7 Mn2 O8 91.7(3) . 2_677 ? O8 Mn2 O8 180.000(3) . 2_677 ? O7 Mn2 O1W 92.2(3) 2_677 . ? O7 Mn2 O1W 87.8(3) . . ? O8 Mn2 O1W 87.5(3) . . ? O8 Mn2 O1W 92.5(3) 2_677 . ? O7 Mn2 O1W 87.8(3) 2_677 2_677 ? O7 Mn2 O1W 92.2(3) . 2_677 ? O8 Mn2 O1W 92.5(3) . 2_677 ? O8 Mn2 O1W 87.5(3) 2_677 2_677 ? O1W Mn2 O1W 180.000(2) . 2_677 ? O5W Na1 O3W 92.2(3) . . ? O5W Na1 O2W 174.8(4) . . ? O3W Na1 O2W 88.8(3) . . ? O5W Na1 O2W 90.0(3) . 2_778 ? O3W Na1 O2W 174.7(4) . 2_778 ? O2W Na1 O2W 88.6(3) . 2_778 ? O5W Na1 O4W 84.5(3) . . ? O3W Na1 O4W 83.4(3) . . ? O2W Na1 O4W 90.6(3) . . ? O2W Na1 O4W 92.0(3) 2_778 . ? O5W Na1 O4 99.1(3) . . ? O3W Na1 O4 97.6(3) . . ? O2W Na1 O4 85.8(3) . . ? O2W Na1 O4 86.8(3) 2_778 . ? O4W Na1 O4 176.2(3) . . ? O5W Na1 Na1 134.0(3) . 2_778 ? O3W Na1 Na1 133.0(3) . 2_778 ? O2W Na1 Na1 44.4(2) . 2_778 ? O2W Na1 Na1 44.2(2) 2_778 2_778 ? O4W Na1 Na1 91.8(3) . 2_778 ? O4 Na1 Na1 84.9(2) . 2_778 ? O6W Na2 O8W 92.3(4) . . ? O6W Na2 O7W 92.1(4) . . ? O8W Na2 O7W 90.1(4) . . ? O6W Na2 O9W 105.7(4) . . ? O8W Na2 O9W 79.2(3) . . ? O7W Na2 O9W 159.4(4) . . ? O6W Na2 O6 172.4(4) . 2_777 ? O8W Na2 O6 80.2(3) . 2_777 ? O7W Na2 O6 87.1(3) . 2_777 ? O9W Na2 O6 73.9(3) . 2_777 ? O6W Na2 O10 123.8(4) . 2_777 ? O8W Na2 O10 142.1(3) . 2_777 ? O7W Na2 O10 98.7(4) . 2_777 ? O9W Na2 O10 80.1(3) . 2_777 ? O6 Na2 O10 63.7(2) 2_777 2_777 ? O6W Na2 Na3 127.1(3) . . ? O8W Na2 Na3 44.5(3) . . ? O7W Na2 Na3 112.3(3) . . ? O9W Na2 Na3 48.4(3) . . ? O6 Na2 Na3 47.0(2) 2_777 . ? O10 Na2 Na3 98.9(2) 2_777 . ? O6W Na2 W4 158.0(4) . 2_777 ? O8W Na2 W4 109.7(3) . 2_777 ? O7W Na2 W4 89.6(3) . 2_777 ? O9W Na2 W4 77.8(2) . 2_777 ? O6 Na2 W4 29.57(15) 2_777 2_777 ? O10 Na2 W4 34.42(15) 2_777 2_777 ? Na3 Na2 W4 71.73(15) . 2_777 ? O6W Na2 W2 94.7(3) . . ? O8W Na2 W2 170.9(3) . . ? O7W Na2 W2 95.6(3) . . ? O9W Na2 W2 93.2(3) . . ? O6 Na2 W2 92.90(19) 2_777 . ? O10 Na2 W2 29.74(15) 2_777 . ? Na3 Na2 W2 126.36(17) . . ? W4 Na2 W2 63.33(8) 2_777 . ? O8W Na3 O10W 172.0(5) . . ? O8W Na3 O7W 88.8(4) . 2_787 ? O10W Na3 O7W 97.8(4) . 2_787 ? O8W Na3 O6 81.5(3) . 2_777 ? O10W Na3 O6 101.6(4) . 2_777 ? O7W Na3 O6 99.6(4) 2_787 2_777 ? O8W Na3 O9W 78.1(4) . . ? O10W Na3 O9W 95.6(4) . . ? O7W Na3 O9W 166.1(4) 2_787 . ? O6 Na3 O9W 74.1(3) 2_777 . ? O8W Na3 O3 82.1(3) . 1_565 ? O10W Na3 O3 95.9(4) . 1_565 ? O7W Na3 O3 70.4(3) 2_787 1_565 ? O6 Na3 O3 161.0(3) 2_777 1_565 ? O9W Na3 O3 111.7(4) . 1_565 ? O8W Na3 Na2 44.5(2) . . ? O10W Na3 Na2 133.1(4) . . ? O7W Na3 Na2 119.6(3) 2_787 . ? O6 Na3 Na2 48.5(2) 2_777 . ? O9W Na3 Na2 47.0(3) . . ? O3 Na3 Na2 121.5(3) 1_565 . ? W3 O3 Na3 122.9(3) . 1_545 ? W4 O4 Na1 147.1(4) . . ? W3 O5 W4 145.5(3) . 2_777 ? W4 O6 Na3 140.4(4) . 2_777 ? W4 O6 Na2 105.2(3) . 2_777 ? Na3 O6 Na2 84.5(3) 2_777 2_777 ? W1 O7 Mn2 140.1(4) . . ? W2 O8 Mn2 138.1(4) . . ? W3 O9 W4 146.9(3) . . ? W2 O10 W4 150.9(4) 2_777 . ? W2 O10 Na2 106.8(3) 2_777 2_777 ? W4 O10 Na2 96.7(3) . 2_777 ? W1 O11 W4 152.0(4) . . ? W2 O12 W1 113.7(3) . . ? W2 O12 Mn1 100.6(3) . . ? W1 O12 Mn1 101.0(3) . . ? W3 O13 Mn1 99.7(3) . . ? W3 O13 W2 114.1(3) . . ? Mn1 O13 W2 99.4(3) . . ? W3 O14 Mn1 99.5(3) . . ? W3 O14 W1 114.3(3) . . ? Mn1 O14 W1 100.8(3) . . ? W1 O15 W2 98.6(2) . . ? W1 O15 W3 99.5(2) . . ? W2 O15 W3 99.0(2) . . ? O18 C1 Mn1 175.7(10) . . ? O17 C2 Mn1 177.3(11) . . ? O16 C3 Mn1 178.5(10) . . ? Na1 O2W Na1 91.4(3) . 2_778 ? Na2 O7W Na3 126.6(5) . 2_787 ? Na2 O8W Na3 90.9(3) . . ? Na2 O9W Na3 84.6(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 3.339 _refine_diff_density_min -1.936 _refine_diff_density_rms 0.290 data_njy2 _database_code_depnum_ccdc_archive 'CCDC 809239' #TrackingRef '- 809237-809239.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H48 Na6 O58 Re2 W8' _chemical_formula_weight 3029.55 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.443(6) _cell_length_b 12.053(8) _cell_length_c 13.891(9) _cell_angle_alpha 72.176(10) _cell_angle_beta 88.395(10) _cell_angle_gamma 71.095(11) _cell_volume 1419.4(16) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2136 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.84 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 20.549 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1193 _exptl_absorpt_correction_T_max 0.2592 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6446 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_av_sigmaI/netI 0.1824 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4808 _reflns_number_gt 2728 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens notdet _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4808 _refine_ls_number_parameters 356 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.1671 _refine_ls_R_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.2735 _refine_ls_wR_factor_gt 0.2141 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.57438(17) 0.64190(15) 0.88088(11) 0.0177(4) Uani 1 1 d U . . W2 W 0.36037(18) 0.57164(17) 0.72952(12) 0.0234(5) Uani 1 1 d . . . W3 W 0.19766(18) 0.78849(17) 0.83809(12) 0.0244(5) Uani 1 1 d . . . W4 W 0.35041(18) 0.69121(16) 1.09926(11) 0.0219(5) Uani 1 1 d . . . Re1 Re 0.4321(2) 0.83105(17) 0.66568(12) 0.0281(5) Uani 1 1 d . . . O1 O 0.725(3) 0.695(3) 0.862(2) 0.031(7) Uani 1 1 d U . . O2 O 0.198(3) 0.538(3) 0.745(2) 0.044(8) Uani 1 1 d U . . O3 O 0.052(3) 0.733(3) 0.842(3) 0.049(9) Uani 1 1 d U . . O4 O 0.203(3) 0.692(3) 1.1717(19) 0.025(6) Uani 1 1 d U . . O5 O 0.657(3) 0.478(3) 0.9170(19) 0.022(6) Uani 1 1 d U . . O6 O 0.391(3) 0.580(3) 0.604(2) 0.032(7) Uani 1 1 d U . . O7 O 0.112(3) 0.945(3) 0.788(2) 0.042(8) Uani 1 1 d . . . O8 O 0.385(3) 0.821(3) 1.104(2) 0.036(8) Uani 1 1 d . . . O9 O 0.531(2) 0.655(2) 1.0043(17) 0.014(5) Uani 1 1 d U . . O10 O 0.229(3) 0.767(3) 0.973(2) 0.027(6) Uani 1 1 d U . . O11 O 0.497(3) 0.425(2) 0.7937(18) 0.017(5) Uani 1 1 d U . . O12 O 0.536(3) 0.640(2) 0.7415(18) 0.016(5) Uani 1 1 d U . . O13 O 0.412(3) 0.803(2) 0.8226(18) 0.018(6) Uani 1 1 d U . . O14 O 0.254(3) 0.754(3) 0.706(2) 0.031(7) Uani 1 1 d . . . O15 O 0.355(3) 0.601(2) 0.8781(18) 0.015(5) Uani 1 1 d U . . O16 O 0.715(4) 0.894(4) 0.634(3) 0.067(11) Uani 1 1 d U . . O17 O 0.431(4) 0.834(3) 0.448(3) 0.055(9) Uani 1 1 d U . . O18 O 0.251(4) 1.099(4) 0.590(3) 0.073(13) Uani 1 1 d . . . C1 C 0.609(5) 0.871(4) 0.651(3) 0.029(10) Uani 1 1 d . . . C2 C 0.426(5) 0.836(5) 0.528(4) 0.043(12) Uani 1 1 d U . . C3 C 0.322(5) 1.000(5) 0.619(3) 0.032(10) Uani 1 1 d U . . Na1 Na 0.317(2) 1.033(2) 1.0202(16) 0.052(5) Uani 1 1 d . . . Na2 Na 0.124(3) 0.647(2) 1.334(2) 0.077(7) Uani 1 1 d . . . Na3 Na -0.038(3) 0.600(3) 0.802(2) 0.099(11) Uani 1 1 d . . . O1W O 0.334(3) 0.838(3) 1.283(2) 0.033(7) Uani 1 1 d U . . O2W O 0.455(4) 0.976(4) 0.891(2) 0.053(10) Uani 1 1 d . . . O3W O 0.817(4) 0.561(4) 0.681(3) 0.068(11) Uani 1 1 d U . . O4W O -0.223(4) 0.944(4) 0.828(2) 0.056(10) Uani 1 1 d . . . O5W O 0.358(5) 0.626(4) 0.395(3) 0.084(14) Uani 1 1 d . . . O6W O 0.077(5) 1.076(4) 0.937(3) 0.078(13) Uani 1 1 d . . . O7W O 0.582(5) 0.798(4) 1.267(3) 0.079(13) Uani 1 1 d . . . O8W O 0.277(4) 1.248(4) 0.926(3) 0.060(11) Uani 1 1 d . . . O9W O 0.098(6) 0.852(4) 1.338(3) 0.094(15) Uani 1 1 d . . . O10W O -0.010(6) 0.423(5) 0.937(4) 0.109(17) Uani 1 1 d U . . O11W O 0.045(6) 0.855(5) 0.543(4) 0.111(17) Uiso 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 W1 0.0190(7) 0.0230(8) 0.0125(7) -0.0031(6) 0.0102(5) -0.0120(6) W2 0.0300(10) 0.0335(11) 0.0130(9) -0.0081(8) 0.0120(7) -0.0188(9) W3 0.0270(10) 0.0352(12) 0.0137(9) -0.0085(8) 0.0108(7) -0.0138(9) W4 0.0292(10) 0.0314(11) 0.0104(8) -0.0083(8) 0.0151(6) -0.0166(8) Re1 0.0459(11) 0.0354(12) 0.0081(8) -0.0035(8) 0.0139(7) -0.0244(9) O1 0.032(10) 0.027(10) 0.032(10) -0.004(8) 0.022(8) -0.016(8) O2 0.035(11) 0.049(12) 0.053(12) -0.013(9) 0.007(8) -0.024(9) O3 0.039(11) 0.053(12) 0.054(12) -0.015(9) 0.015(8) -0.016(9) O4 0.027(10) 0.034(10) 0.015(10) -0.001(8) 0.008(7) -0.017(8) O5 0.016(9) 0.030(10) 0.020(10) -0.006(8) 0.004(7) -0.008(8) O6 0.037(10) 0.041(11) 0.024(10) -0.018(8) 0.005(8) -0.013(8) O7 0.037(19) 0.04(2) 0.05(2) -0.025(18) 0.006(15) -0.002(16) O8 0.06(2) 0.029(19) 0.031(18) -0.013(15) 0.012(15) -0.028(17) O9 0.014(5) 0.014(5) 0.014(5) -0.0042(19) 0.0012(11) -0.005(2) O10 0.034(10) 0.027(10) 0.024(10) -0.016(8) 0.009(7) -0.009(8) O11 0.017(5) 0.017(5) 0.017(5) -0.0052(19) 0.0015(11) -0.006(2) O12 0.016(5) 0.017(5) 0.016(5) -0.0051(19) 0.0015(11) -0.005(2) O13 0.022(9) 0.019(10) 0.015(9) 0.004(7) 0.001(7) -0.017(8) O14 0.015(15) 0.025(17) 0.05(2) -0.016(16) 0.019(13) 0.001(13) O15 0.015(5) 0.015(5) 0.015(5) -0.0046(19) 0.0014(11) -0.005(2) O16 0.067(14) 0.069(14) 0.072(14) -0.014(9) 0.006(9) -0.037(10) O17 0.066(13) 0.058(13) 0.044(13) -0.020(9) 0.004(9) -0.020(9) O18 0.03(2) 0.06(3) 0.09(3) -0.02(3) 0.02(2) 0.02(2) C1 0.04(3) 0.04(3) 0.01(2) 0.00(2) 0.008(17) -0.03(2) C2 0.045(15) 0.046(15) 0.040(15) -0.015(10) 0.003(9) -0.016(10) C3 0.034(13) 0.037(14) 0.023(13) -0.008(9) 0.002(9) -0.010(10) Na1 0.053(13) 0.055(14) 0.053(13) -0.020(11) 0.024(10) -0.026(11) Na2 0.068(16) 0.08(2) 0.09(2) -0.019(16) 0.002(13) -0.035(15) Na3 0.081(19) 0.14(3) 0.15(3) -0.10(2) 0.072(18) -0.09(2) O1W 0.030(10) 0.038(11) 0.025(10) -0.001(8) 0.004(8) -0.013(8) O2W 0.07(2) 0.08(3) 0.012(16) -0.001(17) -0.007(15) -0.04(2) O3W 0.066(14) 0.069(14) 0.068(14) -0.023(10) 0.017(9) -0.022(10) O4W 0.06(2) 0.08(3) 0.03(2) -0.02(2) 0.006(16) -0.01(2) O5W 0.10(3) 0.12(4) 0.03(2) -0.02(3) 0.01(2) -0.03(3) O6W 0.08(3) 0.06(3) 0.09(3) -0.01(3) -0.02(2) -0.03(2) O7W 0.08(3) 0.08(3) 0.08(3) 0.01(3) 0.01(2) -0.06(3) O8W 0.06(2) 0.08(3) 0.06(2) -0.02(2) 0.006(18) -0.04(2) O9W 0.13(4) 0.06(3) 0.07(3) 0.00(3) 0.00(3) -0.02(3) O10W 0.105(19) 0.114(19) 0.105(19) -0.030(11) 0.010(10) -0.035(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 W1 O1 1.72(2) . ? W1 O5 1.78(3) . ? W1 O9 1.79(2) . ? W1 O13 1.98(3) . ? W1 O12 1.99(2) . ? W1 O15 2.28(2) . ? W1 Re1 3.163(3) . ? W1 Na3 3.71(2) 1_655 ? W2 O2 1.70(3) . ? W2 O6 1.74(3) . ? W2 O11 1.79(3) . ? W2 O14 2.03(3) . ? W2 O12 2.11(2) . ? W2 O15 2.19(2) . ? W3 O3 1.70(3) . ? W3 O7 1.72(3) . ? W3 O10 1.84(3) . ? W3 O14 2.02(3) . ? W3 O13 2.09(2) . ? W3 O15 2.18(3) . ? W4 O4 1.69(2) . ? W4 O8 1.71(3) . ? W4 O10 1.91(3) . ? W4 O11 1.95(2) 2_667 ? W4 O9 2.14(2) . ? W4 O5 2.15(3) 2_667 ? Re1 C3 1.87(5) . ? Re1 C1 1.88(4) . ? Re1 C2 1.90(5) . ? Re1 O13 2.11(2) . ? Re1 O12 2.12(3) . ? Re1 O14 2.15(3) . ? O1 Na3 2.41(4) 1_655 ? O2 Na3 2.31(4) . ? O3 Na3 2.26(4) . ? O4 Na2 2.32(4) . ? O5 W4 2.15(3) 2_667 ? O8 Na1 2.34(4) . ? O11 W4 1.95(2) 2_667 ? O16 C1 1.12(5) . ? O17 C2 1.12(5) . ? O18 C3 1.11(6) . ? Na1 O4W 2.33(4) 2_577 ? Na1 O2W 2.33(4) . ? Na1 O6W 2.41(4) . ? Na1 O8W 2.42(4) . ? Na1 O2W 2.46(3) 2_677 ? Na1 Na1 3.35(4) 2_677 ? Na2 O5W 2.30(5) 1_556 ? Na2 O9W 2.42(5) . ? Na2 O3W 2.46(5) 2_667 ? Na3 O10W 2.31(6) . ? Na3 O1 2.41(4) 1_455 ? Na3 O3W 2.44(5) 1_455 ? Na3 W1 3.71(2) 1_455 ? O2W Na1 2.46(3) 2_677 ? O3W Na3 2.44(5) 1_655 ? O3W Na2 2.46(5) 2_667 ? O4W Na1 2.33(4) 2_577 ? O5W Na2 2.30(5) 1_554 ? 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 O1 W1 O5 104.1(12) . . ? O1 W1 O9 100.2(12) . . ? O5 W1 O9 98.1(11) . . ? O1 W1 O13 98.4(12) . . ? O5 W1 O13 155.2(9) . . ? O9 W1 O13 88.0(10) . . ? O1 W1 O12 99.6(12) . . ? O5 W1 O12 87.8(11) . . ? O9 W1 O12 157.3(9) . . ? O13 W1 O12 78.1(10) . . ? O1 W1 O15 169.4(12) . . ? O5 W1 O15 83.6(10) . . ? O9 W1 O15 85.8(9) . . ? O13 W1 O15 72.8(9) . . ? O12 W1 O15 73.1(9) . . ? O1 W1 Re1 87.8(10) . . ? O5 W1 Re1 128.9(8) . . ? O9 W1 Re1 128.9(8) . . ? O13 W1 Re1 41.0(7) . . ? O12 W1 Re1 41.1(7) . . ? O15 W1 Re1 81.6(6) . . ? O1 W1 Na3 31.4(10) . 1_655 ? O5 W1 Na3 77.2(9) . 1_655 ? O9 W1 Na3 120.1(8) . 1_655 ? O13 W1 Na3 120.3(8) . 1_655 ? O12 W1 Na3 82.6(8) . 1_655 ? O15 W1 Na3 149.4(7) . 1_655 ? Re1 W1 Na3 92.1(6) . 1_655 ? O2 W2 O6 102.8(14) . . ? O2 W2 O11 101.7(14) . . ? O6 W2 O11 100.7(12) . . ? O2 W2 O14 93.0(14) . . ? O6 W2 O14 97.4(13) . . ? O11 W2 O14 153.3(11) . . ? O2 W2 O12 163.0(13) . . ? O6 W2 O12 91.7(11) . . ? O11 W2 O12 83.8(10) . . ? O14 W2 O12 76.2(10) . . ? O2 W2 O15 91.6(12) . . ? O6 W2 O15 163.3(11) . . ? O11 W2 O15 84.3(10) . . ? O14 W2 O15 73.1(11) . . ? O12 W2 O15 72.9(9) . . ? O3 W3 O7 102.9(16) . . ? O3 W3 O10 99.9(14) . . ? O7 W3 O10 102.5(13) . . ? O3 W3 O14 90.9(13) . . ? O7 W3 O14 97.5(13) . . ? O10 W3 O14 154.5(12) . . ? O3 W3 O13 161.2(14) . . ? O7 W3 O13 92.7(12) . . ? O10 W3 O13 86.7(10) . . ? O14 W3 O13 76.5(10) . . ? O3 W3 O15 89.9(13) . . ? O7 W3 O15 164.7(12) . . ? O10 W3 O15 83.3(10) . . ? O14 W3 O15 73.6(10) . . ? O13 W3 O15 73.3(9) . . ? O4 W4 O8 101.5(13) . . ? O4 W4 O10 94.6(12) . . ? O8 W4 O10 96.5(13) . . ? O4 W4 O11 95.9(11) . 2_667 ? O8 W4 O11 96.0(12) . 2_667 ? O10 W4 O11 161.7(10) . 2_667 ? O4 W4 O9 167.8(11) . . ? O8 W4 O9 90.7(12) . . ? O10 W4 O9 83.8(10) . . ? O11 W4 O9 82.8(9) 2_667 . ? O4 W4 O5 87.8(11) . 2_667 ? O8 W4 O5 170.5(12) . 2_667 ? O10 W4 O5 84.6(10) . 2_667 ? O11 W4 O5 80.9(9) 2_667 2_667 ? O9 W4 O5 80.0(9) . 2_667 ? C3 Re1 C1 89(2) . . ? C3 Re1 C2 86(2) . . ? C1 Re1 C2 90.5(18) . . ? C3 Re1 O13 98.1(15) . . ? C1 Re1 O13 100.0(13) . . ? C2 Re1 O13 168.6(15) . . ? C3 Re1 O12 169.9(15) . . ? C1 Re1 O12 96.4(16) . . ? C2 Re1 O12 101.9(17) . . ? O13 Re1 O12 72.6(10) . . ? C3 Re1 O14 100.5(15) . . ? C1 Re1 O14 168.9(16) . . ? C2 Re1 O14 95.8(16) . . ? O13 Re1 O14 73.1(10) . . ? O12 Re1 O14 73.4(10) . . ? C3 Re1 W1 134.1(13) . . ? C1 Re1 W1 87.8(13) . . ? C2 Re1 W1 139.3(16) . . ? O13 Re1 W1 38.0(7) . . ? O12 Re1 W1 38.2(6) . . ? O14 Re1 W1 81.5(8) . . ? W1 O1 Na3 126.7(16) . 1_655 ? W2 O2 Na3 142.6(19) . . ? W3 O3 Na3 147(2) . . ? W4 O4 Na2 146.8(16) . . ? W1 O5 W4 146.9(13) . 2_667 ? W4 O8 Na1 141.8(17) . . ? W1 O9 W4 143.4(12) . . ? W3 O10 W4 151.6(16) . . ? W2 O11 W4 155.0(13) . 2_667 ? W1 O12 W2 113.0(11) . . ? W1 O12 Re1 100.7(10) . . ? W2 O12 Re1 101.3(10) . . ? W1 O13 W3 113.1(11) . . ? W1 O13 Re1 101.0(11) . . ? W3 O13 Re1 101.6(9) . . ? W3 O14 W2 111.1(14) . . ? W3 O14 Re1 102.4(12) . . ? W2 O14 Re1 102.6(11) . . ? W3 O15 W2 99.6(10) . . ? W3 O15 W1 99.1(9) . . ? W2 O15 W1 99.4(9) . . ? O16 C1 Re1 174(4) . . ? O17 C2 Re1 176(5) . . ? O18 C3 Re1 177(4) . . ? O4W Na1 O2W 167.7(17) 2_577 . ? O4W Na1 O8 85.5(14) 2_577 . ? O2W Na1 O8 85.3(13) . . ? O4W Na1 O6W 94.9(16) 2_577 . ? O2W Na1 O6W 94.9(15) . . ? O8 Na1 O6W 101.5(14) . . ? O4W Na1 O8W 99.4(15) 2_577 . ? O2W Na1 O8W 89.1(14) . . ? O8 Na1 O8W 173.2(14) . . ? O6W Na1 O8W 82.8(14) . . ? O4W Na1 O2W 79.9(13) 2_577 2_677 ? O2W Na1 O2W 91.4(11) . 2_677 ? O8 Na1 O2W 86.3(13) . 2_677 ? O6W Na1 O2W 170.3(17) . 2_677 ? O8W Na1 O2W 89.9(13) . 2_677 ? O4W Na1 Na1 123.5(14) 2_577 2_677 ? O2W Na1 Na1 47.3(8) . 2_677 ? O8 Na1 Na1 84.0(11) . 2_677 ? O6W Na1 Na1 141.6(15) . 2_677 ? O8W Na1 Na1 89.4(12) . 2_677 ? O2W Na1 Na1 44.1(9) 2_677 2_677 ? O5W Na2 O4 88.4(14) 1_556 . ? O5W Na2 O9W 76.4(18) 1_556 . ? O4 Na2 O9W 90.7(16) . . ? O5W Na2 O3W 97.8(17) 1_556 2_667 ? O4 Na2 O3W 83.3(14) . 2_667 ? O9W Na2 O3W 171.9(19) . 2_667 ? O3 Na3 O2 82.0(13) . . ? O3 Na3 O10W 113(2) . . ? O2 Na3 O10W 97(2) . . ? O3 Na3 O1 88.5(14) . 1_455 ? O2 Na3 O1 170.2(15) . 1_455 ? O10W Na3 O1 88.3(17) . 1_455 ? O3 Na3 O3W 148(2) . 1_455 ? O2 Na3 O3W 99.9(15) . 1_455 ? O10W Na3 O3W 98.9(18) . 1_455 ? O1 Na3 O3W 87.0(14) 1_455 1_455 ? O3 Na3 W1 110.0(12) . 1_455 ? O2 Na3 W1 167.9(12) . 1_455 ? O10W Na3 W1 76.9(14) . 1_455 ? O1 Na3 W1 21.9(7) 1_455 1_455 ? O3W Na3 W1 70.9(10) 1_455 1_455 ? Na1 O2W Na1 88.6(11) . 2_677 ? Na3 O3W Na2 121(2) 1_655 2_667 ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 6.063 _refine_diff_density_min -6.414 _refine_diff_density_rms 0.728