Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr. May Nyman' _publ_contact_author_address ;Sandia National Laboratories Geochemistry Department P.O. BOX 5800, MS 0754 Albuquerque, NM, 87185-0754, USA ; _publ_contact_author_email mdnyman@sandia.gov _publ_contact_author_phone '505 284 4484' _publ_contact_author_fax '505 844 7354' _publ_section_title ; An Aqueous Route to [Ta6O19]8- and Solid-State Studies of Isostructural Niobium and Tantalum Oxide Complexes ; loop_ _publ_author_name 'May Nyman' 'Todd M. Alam' 'Travis M. Anderson' 'Francoise Bonhomme' 'Mark A. Rodriguez' data_HNa7Nb6 _database_code_depnum_ccdc_archive 'CCDC 648089' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common 'heptasodium hexaniobate' _chemical_melting_point ? _chemical_formula_moiety '2(H Nb6 O19) (14 Na) (30 H2O)' _chemical_formula_sum 'H62 Na14 Nb12 O68' _chemical_formula_weight 2587.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P m n n' _symmetry_space_group_name_Hall '-P 2n 2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x, -y, -z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x, y, z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0632(5) _cell_length_b 12.1301(7) _cell_length_c 12.6705(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1546.66(15) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 2.369 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5178 _exptl_absorpt_correction_T_max 0.8240 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS Smart-CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10764 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0133 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.26 _reflns_number_total 1489 _reflns_number_gt 1447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.054 (Bruker, 1998)' _computing_cell_refinement 'SMART 5.054 (Bruker, 1998)' _computing_data_reduction 'SAINT+ 6.22 (Bruker, 2001)' _computing_structure_solution SIR97 _computing_structure_refinement 'XSHELL 4.02 (Bruker, 2000)' _computing_molecular_graphics 'SHELXTL 6.10 (Bruker, 2000)' _computing_publication_material 'SHELXTL 6.10 (Bruker, 2000)' _publ_section_references ; Bruker AXS, Inc. (1998). SMART Version 5.054 Madison, WI 53711-5373 Bruker AXS, Inc. (2000). XSHELL Version 4.01 and SHELXTL Version 6.10. Madison, WI 53711-5373. Bruker AXS, Inc. (2001). SAINT+ Version 6.02. Madison, WI 53711-5373 Sheldrick, G. M. (1999). SADABS Version 2.03. University of Gottingen, Germany. ; _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. The following 9 restraints were employed for structure (1). DFIX 1.34 0.02 H111 H111_ 99 DFIX 1.34 0.02 H121 H122 H131 H132 DFIX 0.82 0.02 O13 H131 O13 H132 DFIX 0.82 0.02 O10 H101 O11 H111 O12 H121 O12 H122 EQIV 99 1-x, y, z These are O-H and H-H bond distance restraints to model the H atoms on the water molecules (O10, O11, O12, O13). Since these bond lengths are well known for water but difficult to observe via X-rays due to low scatter of H atoms, the restraints are a reasonable application to model the H2O coordination. The EQIV command was necessary to establish restraint of the H111 atom for observation of the correct H-O-H bond angle. ; _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^)+(0.0260P)^2^+1.3250P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00239(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1489 _refine_ls_number_parameters 150 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0173 _refine_ls_R_factor_gt 0.0165 _refine_ls_wR_factor_ref 0.0483 _refine_ls_wR_factor_gt 0.0479 _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_restrained_S_all 1.215 _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 Nb1 Nb 0.67102(2) 0.633336(18) 0.028530(16) 0.01041(10) Uani 1 1 d . . . Nb2 Nb 0.5000 0.45706(2) 0.18234(2) 0.00879(11) Uani 1 2 d S . . Na1 Na 0.5000 0.73067(12) 0.24401(11) 0.0177(3) Uani 1 2 d S . . Na2 Na 0.5000 0.99981(12) 0.18764(11) 0.0171(3) Uani 1 2 d S . . Na3 Na 0.5000 1.21612(12) 0.34025(12) 0.0183(3) Uani 1 2 d S . . Na4 Na 0.5000 0.5000 0.5000 0.0329(6) Uani 1 4 d S . . O1 O 0.5000 0.5000 0.0000 0.0103(7) Uani 1 4 d S . . O2 O 0.5000 0.4166(2) 0.31577(18) 0.0155(5) Uani 1 2 d S . . O3 O 0.7781(2) 0.5000 0.0000 0.0118(5) Uani 1 2 d S . . O4 O 0.79590(18) 0.73430(15) 0.05219(14) 0.0160(4) Uani 1 1 d . . . O5 O 0.63441(17) 0.57932(14) 0.17323(12) 0.0111(3) Uani 1 1 d . . . O6 O 0.63868(17) 0.64489(13) -0.12516(13) 0.0116(4) Uani 1 1 d . . . O7 O 0.5000 0.7256(2) 0.04726(19) 0.0120(5) Uani 1 2 d S . . O10 O 0.5000 1.0204(2) 0.3711(2) 0.0197(6) Uani 1 2 d SD . . O11 O 0.5000 0.6895(2) 0.4230(2) 0.0227(6) Uani 1 2 d SD . . O12 O 0.6576(2) 1.14091(17) 0.19625(19) 0.0286(5) Uani 1 1 d D . . O13 O 0.66721(17) 0.86367(16) 0.21707(17) 0.0188(4) Uani 1 1 d D . . O14 O 0.2680(13) 0.5338(13) 0.4881(17) 0.032(3) Uiso 0.25 1 d P . . O14' O 0.2744(12) 0.510(2) 0.5176(12) 0.032(4) Uiso 0.25 1 d P . . O15 O 0.5000 1.0535(5) -0.0057(5) 0.0415(18) Uani 0.50 2 d SP . . H101 H 0.566(2) 1.006(2) 0.405(2) 0.031(4) Uiso 1 1 d D . . H111 H 0.5659(10) 0.710(3) 0.457(2) 0.031(4) Uiso 1 1 d D . . H121 H 0.724(2) 1.126(2) 0.232(2) 0.031(4) Uiso 1 1 d D . . H122 H 0.665(3) 1.1999(18) 0.168(2) 0.031(4) Uiso 1 1 d D . . H131 H 0.717(3) 0.876(3) 0.2677(18) 0.031(4) Uiso 1 1 d D . . H132 H 0.709(3) 0.836(3) 0.1704(18) 0.031(4) Uiso 1 1 d 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 Nb1 0.01170(15) 0.01032(15) 0.00922(15) 0.00000(8) -0.00055(8) -0.00358(8) Nb2 0.00965(17) 0.00941(18) 0.00732(17) 0.00058(11) 0.000 0.000 Na1 0.0205(8) 0.0172(7) 0.0154(7) -0.0034(6) 0.000 0.000 Na2 0.0182(8) 0.0155(7) 0.0177(7) -0.0015(6) 0.000 0.000 Na3 0.0185(8) 0.0159(7) 0.0205(8) 0.0002(6) 0.000 0.000 Na4 0.0315(14) 0.0279(13) 0.0393(14) 0.0077(12) 0.000 0.000 O1 0.0117(17) 0.0119(17) 0.0073(16) 0.0010(14) 0.000 0.000 O2 0.0198(14) 0.0146(13) 0.0121(13) 0.0005(10) 0.000 0.000 O3 0.0089(12) 0.0129(12) 0.0136(12) -0.0007(10) 0.000 0.000 O4 0.0160(9) 0.0155(9) 0.0166(9) -0.0001(7) -0.0012(8) -0.0054(8) O5 0.0114(8) 0.0119(8) 0.0098(8) -0.0006(7) -0.0006(7) -0.0014(7) O6 0.0111(8) 0.0142(9) 0.0094(8) 0.0012(7) 0.0011(7) -0.0021(7) O7 0.0113(12) 0.0136(13) 0.0111(12) -0.0009(10) 0.000 0.000 O10 0.0136(14) 0.0288(15) 0.0166(14) 0.0039(12) 0.000 0.000 O11 0.0217(15) 0.0300(16) 0.0164(14) -0.0059(12) 0.000 0.000 O12 0.0257(12) 0.0208(11) 0.0393(14) 0.0145(9) -0.0151(10) -0.0079(9) O13 0.0147(10) 0.0222(11) 0.0195(11) -0.0069(8) -0.0029(8) 0.0022(7) O15 0.088(6) 0.022(3) 0.015(3) 0.003(3) 0.000 0.000 _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 Nb1 O4 1.7801(17) . ? Nb1 O3 1.9766(13) . ? Nb1 O6 1.9793(17) . ? Nb1 O5 1.9815(16) . ? Nb1 O7 2.0669(14) . ? Nb1 O1 2.3892(2) . ? Nb1 Nb1 3.3146(5) 3_565 ? Nb1 Na1 3.4366(12) . ? Nb2 O2 1.761(2) . ? Nb2 O6 2.0005(17) 5_665 ? Nb2 O6 2.0005(17) 3_565 ? Nb2 O5 2.0105(17) . ? Nb2 O5 2.0105(17) 7_655 ? Nb2 O1 2.3683(3) . ? Nb2 Na1 3.4096(14) . ? Nb2 Na3 3.5419(15) 1_545 ? Na1 O11 2.323(3) . ? Na1 O13 2.356(2) . ? Na1 O13 2.356(2) 7_655 ? Na1 O5 2.450(2) 7_655 ? Na1 O5 2.450(2) . ? Na1 O7 2.494(3) . ? Na1 Na2 3.342(2) . ? Na1 Nb1 3.4366(12) 7_655 ? Na1 H132 2.63(3) . ? Na2 O12 2.336(2) . ? Na2 O12 2.336(2) 7_655 ? Na2 O10 2.338(3) . ? Na2 O13 2.387(2) 7_655 ? Na2 O13 2.387(2) . ? Na2 O15 2.394(6) 5_675 ? Na2 O15 2.535(6) . ? Na2 Na3 3.259(2) . ? Na3 O10 2.406(3) . ? Na3 O2 2.451(3) 1_565 ? Na3 O4 2.4748(19) 4_655 ? Na3 O4 2.4748(19) 6_566 ? Na3 O12 2.584(3) 7_655 ? Na3 O12 2.584(3) . ? Na3 Nb2 3.5419(15) 1_565 ? Na3 Na4 3.9944(15) 1_565 ? Na4 O14' 2.285(12) 7_655 ? Na4 O14' 2.285(12) 5_666 ? Na4 O14' 2.285(12) 3_566 ? Na4 O14' 2.285(12) . ? Na4 O14 2.375(14) 7_655 ? Na4 O14 2.375(14) 5_666 ? Na4 O14 2.375(14) . ? Na4 O14 2.375(14) 3_566 ? Na4 O11 2.497(3) . ? Na4 O11 2.497(3) 5_666 ? Na4 O2 2.544(2) 5_666 ? Na4 O2 2.544(2) . ? O1 Nb2 2.3683(3) 5_665 ? O1 Nb1 2.3892(2) 5_665 ? O1 Nb1 2.3892(2) 3_565 ? O1 Nb1 2.3892(2) 7_655 ? O2 Na3 2.451(3) 1_545 ? O3 Nb1 1.9766(13) 3_565 ? O4 Na3 2.4748(19) 6_656 ? O6 Nb2 2.0005(17) 5_665 ? O7 Nb1 2.0669(14) 7_655 ? O10 H101 0.805(18) . ? O11 H111 0.825(15) . ? O12 H121 0.828(17) . ? O12 H122 0.802(17) . ? O13 H131 0.828(17) . ? O13 H132 0.801(17) . ? O14 O14' 0.54(2) 3_566 ? O14 O14 0.88(3) 3_566 ? O14' O14' 0.51(2) 3_566 ? O14' O14 0.54(2) 3_566 ? O15 O15 1.307(12) 5_675 ? O15 Na2 2.394(6) 5_675 ? 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 O4 Nb1 O3 102.06(8) . . ? O4 Nb1 O6 103.48(8) . . ? O3 Nb1 O6 88.15(5) . . ? O4 Nb1 O5 101.71(8) . . ? O3 Nb1 O5 90.00(5) . . ? O6 Nb1 O5 154.58(7) . . ? O4 Nb1 O7 101.29(8) . . ? O3 Nb1 O7 156.65(8) . . ? O6 Nb1 O7 86.43(8) . . ? O5 Nb1 O7 85.30(8) . . ? O4 Nb1 O1 178.57(6) . . ? O3 Nb1 O1 79.11(6) . . ? O6 Nb1 O1 77.33(5) . . ? O5 Nb1 O1 77.42(5) . . ? O7 Nb1 O1 77.54(6) . . ? O4 Nb1 Nb1 135.08(6) . 3_565 ? O3 Nb1 Nb1 33.02(6) . 3_565 ? O6 Nb1 Nb1 81.63(5) . 3_565 ? O5 Nb1 Nb1 83.06(5) . 3_565 ? O7 Nb1 Nb1 123.62(6) . 3_565 ? O1 Nb1 Nb1 46.081(6) . 3_565 ? O4 Nb1 Na1 89.05(6) . . ? O3 Nb1 Na1 134.37(3) . . ? O6 Nb1 Na1 132.45(5) . . ? O5 Nb1 Na1 44.39(5) . . ? O7 Nb1 Na1 46.03(7) . . ? O1 Nb1 Na1 89.544(18) . . ? Nb1 Nb1 Na1 120.57(2) 3_565 . ? O2 Nb2 O6 100.10(8) . 5_665 ? O2 Nb2 O6 100.10(8) . 3_565 ? O6 Nb2 O6 88.47(10) 5_665 3_565 ? O2 Nb2 O5 105.12(8) . . ? O6 Nb2 O5 154.76(7) 5_665 . ? O6 Nb2 O5 88.05(7) 3_565 . ? O2 Nb2 O5 105.12(8) . 7_655 ? O6 Nb2 O5 88.05(7) 5_665 7_655 ? O6 Nb2 O5 154.76(7) 3_565 7_655 ? O5 Nb2 O5 84.56(10) . 7_655 ? O2 Nb2 O1 176.51(8) . . ? O6 Nb2 O1 77.45(5) 5_665 . ? O6 Nb2 O1 77.45(5) 3_565 . ? O5 Nb2 O1 77.39(5) . . ? O5 Nb2 O1 77.39(5) 7_655 . ? O2 Nb2 Na1 92.95(9) . . ? O6 Nb2 Na1 133.22(5) 5_665 . ? O6 Nb2 Na1 133.22(5) 3_565 . ? O5 Nb2 Na1 45.18(5) . . ? O5 Nb2 Na1 45.18(5) 7_655 . ? O1 Nb2 Na1 90.54(3) . . ? O2 Nb2 Na3 39.41(9) . 1_545 ? O6 Nb2 Na3 72.21(5) 5_665 1_545 ? O6 Nb2 Na3 72.21(5) 3_565 1_545 ? O5 Nb2 Na3 129.88(5) . 1_545 ? O5 Nb2 Na3 129.88(5) 7_655 1_545 ? O1 Nb2 Na3 137.10(3) . 1_545 ? Na1 Nb2 Na3 132.36(4) . 1_545 ? O11 Na1 O13 106.78(8) . . ? O11 Na1 O13 106.78(8) . 7_655 ? O13 Na1 O13 91.16(10) . 7_655 ? O11 Na1 O5 101.33(8) . 7_655 ? O13 Na1 O5 148.68(9) . 7_655 ? O13 Na1 O5 93.77(6) 7_655 7_655 ? O11 Na1 O5 101.33(8) . . ? O13 Na1 O5 93.77(6) . . ? O13 Na1 O5 148.68(9) 7_655 . ? O5 Na1 O5 67.01(9) 7_655 . ? O11 Na1 O7 166.19(11) . . ? O13 Na1 O7 82.64(7) . . ? O13 Na1 O7 82.64(7) 7_655 . ? O5 Na1 O7 67.41(7) 7_655 . ? O5 Na1 O7 67.41(7) . . ? O11 Na1 Na2 114.75(9) . . ? O13 Na1 Na2 45.58(5) . . ? O13 Na1 Na2 45.58(5) 7_655 . ? O5 Na1 Na2 130.82(6) 7_655 . ? O5 Na1 Na2 130.82(6) . . ? O7 Na1 Na2 79.06(7) . . ? O11 Na1 Nb2 90.83(8) . . ? O13 Na1 Nb2 129.30(5) . . ? O13 Na1 Nb2 129.30(5) 7_655 . ? O5 Na1 Nb2 35.59(4) 7_655 . ? O5 Na1 Nb2 35.59(4) . . ? O7 Na1 Nb2 75.35(7) . . ? Na2 Na1 Nb2 154.41(5) . . ? O11 Na1 Nb1 134.59(6) . 7_655 ? O13 Na1 Nb1 118.54(7) . 7_655 ? O13 Na1 Nb1 76.26(5) 7_655 7_655 ? O5 Na1 Nb1 34.45(4) 7_655 7_655 ? O5 Na1 Nb1 74.23(5) . 7_655 ? O7 Na1 Nb1 36.62(3) . 7_655 ? Na2 Na1 Nb1 99.55(4) . 7_655 ? Nb2 Na1 Nb1 58.90(2) . 7_655 ? O11 Na1 Nb1 134.59(6) . . ? O13 Na1 Nb1 76.26(5) . . ? O13 Na1 Nb1 118.54(7) 7_655 . ? O5 Na1 Nb1 74.23(5) 7_655 . ? O5 Na1 Nb1 34.45(4) . . ? O7 Na1 Nb1 36.62(3) . . ? Na2 Na1 Nb1 99.55(4) . . ? Nb2 Na1 Nb1 58.90(2) . . ? Nb1 Na1 Nb1 60.11(2) 7_655 . ? O11 Na1 H132 116.8(6) . . ? O13 Na1 H132 17.4(5) . . ? O13 Na1 H132 100.8(7) 7_655 . ? O5 Na1 H132 132.4(4) 7_655 . ? O5 Na1 H132 78.0(6) . . ? O7 Na1 H132 69.9(5) . . ? Na2 Na1 H132 56.7(6) . . ? Nb2 Na1 H132 113.0(5) . . ? Nb1 Na1 H132 106.6(5) 7_655 . ? Nb1 Na1 H132 58.9(4) . . ? O12 Na2 O12 85.53(12) . 7_655 ? O12 Na2 O10 82.83(9) . . ? O12 Na2 O10 82.83(9) 7_655 . ? O12 Na2 O13 168.03(10) . 7_655 ? O12 Na2 O13 91.20(7) 7_655 7_655 ? O10 Na2 O13 85.34(8) . 7_655 ? O12 Na2 O13 91.20(7) . . ? O12 Na2 O13 168.03(10) 7_655 . ? O10 Na2 O13 85.34(8) . . ? O13 Na2 O13 89.65(10) 7_655 . ? O12 Na2 O15 104.06(13) . 5_675 ? O12 Na2 O15 104.06(13) 7_655 5_675 ? O10 Na2 O15 170.46(17) . 5_675 ? O13 Na2 O15 87.90(12) 7_655 5_675 ? O13 Na2 O15 87.90(12) . 5_675 ? O12 Na2 O15 81.77(12) . . ? O12 Na2 O15 81.77(12) 7_655 . ? O10 Na2 O15 158.96(16) . . ? O13 Na2 O15 109.20(11) 7_655 . ? O13 Na2 O15 109.20(11) . . ? O15 Na2 O15 30.6(3) 5_675 . ? O12 Na2 Na3 51.87(7) . . ? O12 Na2 Na3 51.87(7) 7_655 . ? O10 Na2 Na3 47.47(8) . . ? O13 Na2 Na3 117.66(6) 7_655 . ? O13 Na2 Na3 117.66(6) . . ? O15 Na2 Na3 142.07(15) 5_675 . ? O15 Na2 Na3 111.49(15) . . ? O12 Na2 Na1 134.89(6) . . ? O12 Na2 Na1 134.89(6) 7_655 . ? O10 Na2 Na1 83.80(8) . . ? O13 Na2 Na1 44.83(5) 7_655 . ? O13 Na2 Na1 44.83(5) . . ? O15 Na2 Na1 86.66(15) 5_675 . ? O15 Na2 Na1 117.24(14) . . ? Na3 Na2 Na1 131.27(6) . . ? O10 Na3 O2 177.91(11) . 1_565 ? O10 Na3 O4 89.91(7) . 4_655 ? O2 Na3 O4 88.93(6) 1_565 4_655 ? O10 Na3 O4 89.91(7) . 6_566 ? O2 Na3 O4 88.93(6) 1_565 6_566 ? O4 Na3 O4 112.19(10) 4_655 6_566 ? O10 Na3 O12 76.49(8) . 7_655 ? O2 Na3 O12 105.12(8) 1_565 7_655 ? O4 Na3 O12 158.40(8) 4_655 7_655 ? O4 Na3 O12 84.88(6) 6_566 7_655 ? O10 Na3 O12 76.49(8) . . ? O2 Na3 O12 105.12(8) 1_565 . ? O4 Na3 O12 84.88(6) 4_655 . ? O4 Na3 O12 158.40(8) 6_566 . ? O12 Na3 O12 75.74(10) 7_655 . ? O10 Na3 Na2 45.75(7) . . ? O2 Na3 Na2 136.34(8) 1_565 . ? O4 Na3 Na2 113.48(5) 4_655 . ? O4 Na3 Na2 113.48(5) 6_566 . ? O12 Na3 Na2 45.33(5) 7_655 . ? O12 Na3 Na2 45.33(5) . . ? O10 Na3 Nb2 154.96(9) . 1_565 ? O2 Na3 Nb2 27.13(6) 1_565 1_565 ? O4 Na3 Nb2 103.74(6) 4_655 1_565 ? O4 Na3 Nb2 103.74(6) 6_566 1_565 ? O12 Na3 Nb2 83.83(6) 7_655 1_565 ? O12 Na3 Nb2 83.83(6) . 1_565 ? Na2 Na3 Nb2 109.22(5) . 1_565 ? O10 Na3 Na4 140.20(8) . 1_565 ? O2 Na3 Na4 37.71(6) 1_565 1_565 ? O4 Na3 Na4 69.15(5) 4_655 1_565 ? O4 Na3 Na4 69.15(5) 6_566 1_565 ? O12 Na3 Na4 131.46(6) 7_655 1_565 ? O12 Na3 Na4 131.46(6) . 1_565 ? Na2 Na3 Na4 174.06(5) . 1_565 ? Nb2 Na3 Na4 64.84(2) 1_565 1_565 ? O14' Na4 O14' 12.9(6) 7_655 5_666 ? O14' Na4 O14' 180.00(7) 7_655 3_566 ? O14' Na4 O14' 167.1(6) 5_666 3_566 ? O14' Na4 O14' 167.1(6) 7_655 . ? O14' Na4 O14' 180.000(1) 5_666 . ? O14' Na4 O14' 12.9(6) 3_566 . ? O14' Na4 O14 11.5(5) 7_655 7_655 ? O14' Na4 O14 13.2(5) 5_666 7_655 ? O14' Na4 O14 168.5(5) 3_566 7_655 ? O14' Na4 O14 166.8(5) . 7_655 ? O14' Na4 O14 13.2(5) 7_655 5_666 ? O14' Na4 O14 11.5(5) 5_666 5_666 ? O14' Na4 O14 166.8(5) 3_566 5_666 ? O14' Na4 O14 168.5(5) . 5_666 ? O14 Na4 O14 21.2(7) 7_655 5_666 ? O14' Na4 O14 166.8(5) 7_655 . ? O14' Na4 O14 168.5(5) 5_666 . ? O14' Na4 O14 13.2(5) 3_566 . ? O14' Na4 O14 11.5(5) . . ? O14 Na4 O14 158.8(7) 7_655 . ? O14 Na4 O14 180.000(1) 5_666 . ? O14' Na4 O14 168.5(5) 7_655 3_566 ? O14' Na4 O14 166.8(5) 5_666 3_566 ? O14' Na4 O14 11.5(5) 3_566 3_566 ? O14' Na4 O14 13.2(5) . 3_566 ? O14 Na4 O14 180.000(1) 7_655 3_566 ? O14 Na4 O14 158.8(7) 5_666 3_566 ? O14 Na4 O14 21.2(7) . 3_566 ? O14' Na4 O11 89.3(8) 7_655 . ? O14' Na4 O11 90.7(8) 5_666 . ? O14' Na4 O11 90.7(8) 3_566 . ? O14' Na4 O11 89.3(8) . . ? O14 Na4 O11 79.4(3) 7_655 . ? O14 Na4 O11 100.6(3) 5_666 . ? O14 Na4 O11 79.4(3) . . ? O14 Na4 O11 100.6(3) 3_566 . ? O14' Na4 O11 90.7(8) 7_655 5_666 ? O14' Na4 O11 89.3(8) 5_666 5_666 ? O14' Na4 O11 89.3(8) 3_566 5_666 ? O14' Na4 O11 90.7(8) . 5_666 ? O14 Na4 O11 100.6(3) 7_655 5_666 ? O14 Na4 O11 79.4(3) 5_666 5_666 ? O14 Na4 O11 100.6(3) . 5_666 ? O14 Na4 O11 79.4(3) 3_566 5_666 ? O11 Na4 O11 180.00(5) . 5_666 ? O14' Na4 O2 83.6(3) 7_655 5_666 ? O14' Na4 O2 96.4(3) 5_666 5_666 ? O14' Na4 O2 96.4(3) 3_566 5_666 ? O14' Na4 O2 83.6(3) . 5_666 ? O14 Na4 O2 89.4(6) 7_655 5_666 ? O14 Na4 O2 90.6(6) 5_666 5_666 ? O14 Na4 O2 89.4(6) . 5_666 ? O14 Na4 O2 90.6(6) 3_566 5_666 ? O11 Na4 O2 89.55(8) . 5_666 ? O11 Na4 O2 90.45(8) 5_666 5_666 ? O14' Na4 O2 96.4(3) 7_655 . ? O14' Na4 O2 83.6(3) 5_666 . ? O14' Na4 O2 83.6(3) 3_566 . ? O14' Na4 O2 96.4(3) . . ? O14 Na4 O2 90.6(6) 7_655 . ? O14 Na4 O2 89.4(6) 5_666 . ? O14 Na4 O2 90.6(6) . . ? O14 Na4 O2 89.4(6) 3_566 . ? O11 Na4 O2 90.45(8) . . ? O11 Na4 O2 89.55(8) 5_666 . ? O2 Na4 O2 180.0 5_666 . ? Nb2 O1 Nb2 180.000(14) . 5_665 ? Nb2 O1 Nb1 90.073(7) . . ? Nb2 O1 Nb1 89.927(7) 5_665 . ? Nb2 O1 Nb1 89.927(7) . 5_665 ? Nb2 O1 Nb1 90.073(7) 5_665 5_665 ? Nb1 O1 Nb1 180.0 . 5_665 ? Nb2 O1 Nb1 89.927(7) . 3_565 ? Nb2 O1 Nb1 90.073(7) 5_665 3_565 ? Nb1 O1 Nb1 87.838(12) . 3_565 ? Nb1 O1 Nb1 92.162(11) 5_665 3_565 ? Nb2 O1 Nb1 90.073(7) . 7_655 ? Nb2 O1 Nb1 89.927(7) 5_665 7_655 ? Nb1 O1 Nb1 92.162(12) . 7_655 ? Nb1 O1 Nb1 87.838(11) 5_665 7_655 ? Nb1 O1 Nb1 180.000(7) 3_565 7_655 ? Nb2 O2 Na3 113.46(12) . 1_545 ? Nb2 O2 Na4 140.37(13) . . ? Na3 O2 Na4 106.17(9) 1_545 . ? Nb1 O3 Nb1 113.95(11) 3_565 . ? Nb1 O4 Na3 128.12(10) . 6_656 ? Nb1 O5 Nb2 114.97(8) . . ? Nb1 O5 Na1 101.16(8) . . ? Nb2 O5 Na1 99.22(7) . . ? Nb1 O6 Nb2 115.29(8) . 5_665 ? Nb1 O7 Nb1 112.75(11) . 7_655 ? Nb1 O7 Na1 97.35(8) . . ? Nb1 O7 Na1 97.35(8) 7_655 . ? Na2 O10 Na3 86.78(10) . . ? Na2 O10 H101 120(2) . . ? Na3 O10 H101 107(2) . . ? Na1 O11 Na4 125.40(12) . . ? Na1 O11 H111 116(2) . . ? Na4 O11 H111 94(2) . . ? Na2 O12 Na3 82.81(8) . . ? Na2 O12 H121 115(2) . . ? Na3 O12 H121 100(2) . . ? Na2 O12 H122 134(2) . . ? Na3 O12 H122 93(2) . . ? H121 O12 H122 111(2) . . ? Na1 O13 Na2 89.59(7) . . ? Na1 O13 H131 116(2) . . ? Na2 O13 H131 115(2) . . ? Na1 O13 H132 101(2) . . ? Na2 O13 H132 123(2) . . ? H131 O13 H132 109(2) . . ? O14' O14 O14 28.6(18) 3_566 3_566 ? O14' O14 Na4 74(2) 3_566 . ? O14 O14 Na4 79.4(3) 3_566 . ? O14' O14' O14 53(4) 3_566 3_566 ? O14' O14' Na4 83.6(3) 3_566 . ? O14 O14' Na4 93(3) 3_566 . ? O15 O15 Na2 80.7(5) 5_675 5_675 ? O15 O15 Na2 68.7(5) 5_675 . ? Na2 O15 Na2 149.4(3) 5_675 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.417 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.124 # Attachment '2_.cif' data_na8ta6 _database_code_depnum_ccdc_archive 'CCDC 648090' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'octasodium hexatantalate' _chemical_melting_point ? _chemical_formula_moiety '2 (O19 Ta6), 16(Na), 30(H2O)' _chemical_formula_sum 'H60 Na16 O68 Ta12' _chemical_formula_weight 3687.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P m n n' _symmetry_space_group_name_Hall '-P 2n 2' _symmetry_int_tables_number 58 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x, -y, -z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x, y, z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0215(16) _cell_length_b 12.007(2) _cell_length_c 12.761(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1535.5(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.988 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 21.524 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0597 _exptl_absorpt_correction_T_max 0.4125 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS Smart-CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12014 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0137 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.02 _reflns_number_total 1886 _reflns_number_gt 1825 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.054 (Bruker, 1998)' _computing_cell_refinement 'SMART 5.054 (Bruker, 1998)' _computing_data_reduction 'SAINT+ 6.22 (Bruker, 2001)' _computing_structure_solution SIR97 _computing_structure_refinement 'XSHELL 4.02 (Bruker, 2000)' _computing_molecular_graphics 'SHELXTL 6.10 (Bruker, 2000)' _computing_publication_material 'SHELXTL 6.10 (Bruker, 2000)' _publ_section_references ; Bruker AXS, Inc. (1998). SMART Version 5.054 Madison, WI 53711-5373 Bruker AXS, Inc. (2000). XSHELL Version 4.01 and SHELXTL Version 6.10. Madison, WI 53711-5373. Bruker AXS, Inc. (2001). SAINT+ Version 6.02. Madison, WI 53711-5373 Sheldrick, G. M. (1999). SADABS Version 2.03. University of Gottingen, Germany. ; _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. The following 6 restraints were employed for structure (2). DFIX 0.82 0.02 O12 H12a O12 H12b O13 H13a O13 H13b DFIX 1.34 0.02 H12a H12b H13a H13b These are O-H and H-H bond distance restraints to model the H atoms on the water molecules (O12 and O13). Since these bond lengths are well known for water but difficult to observe via X-rays due to low scatter of H atoms, the restraints are a reasonable application to model the H2O coordination. ; _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^)+(0.0336P)^2^+8.2753P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1886 _refine_ls_number_parameters 153 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0198 _refine_ls_R_factor_gt 0.0189 _refine_ls_wR_factor_ref 0.0503 _refine_ls_wR_factor_gt 0.0499 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.140 _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 0.5000 0.7319(2) 0.2415(2) 0.0162(5) Uani 1 2 d S . . Na2 Na 0.5000 0.0026(2) 0.19575(19) 0.0193(5) Uani 1 2 d S . . Na3 Na 0.5000 0.2200(2) 0.3473(2) 0.0163(5) Uani 1 2 d S . . Na4 Na 0.5000 0.5000 0.5000 0.0267(8) Uani 1 4 d S . . Na5 Na 0.6347(9) 0.8953(7) 0.9901(7) 0.0297(17) Uani 0.25 1 d P . . Ta1 Ta 0.666537(16) 0.636040(14) 0.026786(12) 0.00935(7) Uani 1 1 d . . . Ta2 Ta 0.5000 0.459106(18) 0.184077(17) 0.00888(8) Uani 1 2 d S . . O1 O 0.5000 0.5000 0.0000 0.0104(11) Uani 1 4 d S . . O2 O 0.5000 0.4203(4) 0.3194(3) 0.0145(9) Uani 1 2 d S . . O3 O 0.7739(4) 0.5000 0.0000 0.0115(8) Uani 1 2 d S . . O4 O 0.7929(3) 0.7410(2) 0.0495(2) 0.0146(6) Uani 1 1 d . . . O5 O 0.6350(3) 0.5811(2) 0.1716(2) 0.0098(5) Uani 1 1 d . . . O6 O 0.6387(3) 0.3566(2) 0.1269(2) 0.0110(6) Uani 1 1 d . . . O7 O 0.5000 0.7242(3) 0.0428(3) 0.0114(8) Uani 1 2 d S . . O10 O 0.5000 0.0205(4) 0.3757(3) 0.0177(9) Uani 1 2 d S . . O11 O 0.5000 0.6983(4) 0.4201(4) 0.0258(11) Uani 1 2 d S . . O12 O 0.6569(3) 0.1446(3) 0.2022(3) 0.0238(8) Uani 1 1 d D . . O13 O 0.6686(3) 0.8659(3) 0.2144(3) 0.0195(8) Uani 1 1 d D . . O14 O 0.7196(8) 0.5324(6) 0.4812(6) 0.033(2) Uani 0.50 1 d P . . O15 O 0.5000 0.0419(8) 0.9966(9) 0.034(3) Uani 0.50 2 d SP . . H12A H 0.670(6) 0.206(3) 0.175(5) 0.052(11) Uiso 1 1 d D . . H12B H 0.723(5) 0.131(5) 0.241(5) 0.052(11) Uiso 1 1 d D . . H13A H 0.722(5) 0.882(5) 0.262(4) 0.052(11) Uiso 1 1 d D . . H13B H 0.712(5) 0.827(5) 0.172(4) 0.052(11) Uiso 1 1 d 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 Na1 0.0178(12) 0.0136(11) 0.0173(12) -0.0024(9) 0.000 0.000 Na2 0.0141(12) 0.0197(13) 0.0240(13) -0.0039(11) 0.000 0.000 Na3 0.0132(11) 0.0156(12) 0.0202(12) 0.0006(10) 0.000 0.000 Na4 0.0170(18) 0.027(2) 0.036(2) 0.0019(18) 0.000 0.000 Na5 0.039(5) 0.023(4) 0.026(4) 0.000(4) 0.000(4) 0.006(4) Ta1 0.00658(10) 0.00977(11) 0.01171(11) -0.00048(5) 0.00019(5) -0.00157(5) Ta2 0.00685(12) 0.00870(13) 0.01110(13) 0.00060(7) 0.000 0.000 O1 0.007(3) 0.009(3) 0.016(3) 0.000(2) 0.000 0.000 O2 0.015(2) 0.014(2) 0.015(2) -0.0008(16) 0.000 0.000 O3 0.0069(19) 0.014(2) 0.0139(18) 0.0013(16) 0.000 0.000 O4 0.0127(14) 0.0144(15) 0.0166(14) -0.0018(12) 0.0002(12) -0.0043(12) O5 0.0084(12) 0.0103(13) 0.0106(13) -0.0005(10) -0.0007(10) -0.0007(11) O6 0.0089(13) 0.0105(14) 0.0134(15) 0.0014(10) -0.0023(11) 0.0010(10) O7 0.013(2) 0.0076(19) 0.014(2) -0.0016(15) 0.000 0.000 O10 0.012(2) 0.023(2) 0.017(2) 0.0006(18) 0.000 0.000 O11 0.018(2) 0.039(3) 0.020(2) -0.009(2) 0.000 0.000 O12 0.0182(18) 0.0189(18) 0.034(2) 0.0100(15) -0.0104(14) -0.0074(12) O13 0.0134(17) 0.0191(18) 0.026(2) -0.0076(13) -0.0048(13) 0.0034(11) O14 0.029(4) 0.043(6) 0.027(5) -0.012(3) -0.005(3) 0.025(3) O15 0.066(8) 0.016(5) 0.019(5) 0.000(4) 0.000 0.000 _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 O11 2.314(5) . ? Na1 O13 2.359(4) . ? Na1 O13 2.359(4) 7_655 ? Na1 O5 2.429(3) 7_655 ? Na1 Na2 3.303(4) 1_565 ? Na1 Ta1 3.409(2) 7_655 ? Na1 Ta1 3.409(2) . ? Na1 Na5 3.996(9) 7_654 ? Na1 Na5 3.996(9) 1_554 ? Na1 H13B 2.58(7) . ? Na2 O10 2.307(5) . ? Na2 O12 2.320(4) . ? Na2 O12 2.320(4) 7_655 ? Na2 O13 2.368(4) 7_645 ? Na2 O13 2.368(4) 1_545 ? Na2 O15 2.512(12) 5_656 ? Na2 O15 2.585(12) 1_554 ? Na2 Na5 2.992(9) 5_666 ? Na2 Na5 2.992(9) 3_566 ? Na2 Na5 3.220(9) 7_644 ? Na2 Na5 3.220(9) 1_544 ? Na2 Na3 3.249(4) . ? Na3 O10 2.423(5) . ? Na3 O2 2.432(5) . ? Na3 O4 2.470(3) 4_645 ? Na3 O4 2.470(3) 6_556 ? Na3 O12 2.593(5) 7_655 ? Na3 O12 2.593(5) . ? Na3 Ta2 3.547(3) . ? Na3 Na4 3.886(3) . ? Na4 O14 2.247(8) . ? Na4 O14 2.247(8) 7_655 ? Na4 O14 2.247(8) 5_666 ? Na4 O14 2.247(8) 3_566 ? Na4 O2 2.495(4) 5_666 ? Na4 O11 2.590(5) . ? Na4 O11 2.590(5) 5_666 ? Na4 Na5 3.873(10) 2_664 ? Na4 Na5 3.873(10) 6_557 ? Na4 Na5 3.873(10) 8_575 ? Na4 Na5 3.873(10) 4_646 ? Na4 Na3 3.886(3) 5_666 ? Na5 O15 1.555(10) 5_667 ? Na5 O14 1.703(13) 2_665 ? Na5 O15 2.219(12) 1_565 ? Na5 O14 2.230(12) 4_656 ? Na5 O12 2.510(10) 3_566 ? Na5 Na5 2.526(18) 3_577 ? Na5 O7 2.549(10) 1_556 ? Na5 O4 2.554(9) 1_556 ? Na5 Na5 2.700(19) 7_655 ? Na5 O13 2.904(10) 1_556 ? Na5 Na2 2.992(9) 5_666 ? Na5 Ta1 3.164(9) 1_556 ? Ta1 O4 1.810(3) . ? Ta1 O6 1.983(3) 3_565 ? Ta1 O3 1.985(2) . ? Ta1 O7 1.987(2) . ? Ta1 O5 1.988(3) . ? Ta1 O1 2.3602(3) . ? Ta1 Na5 3.164(9) 1_554 ? Ta1 Ta1 3.3377(6) 3_565 ? Ta1 Ta1 3.3379(6) 7_655 ? Ta2 O2 1.788(4) . ? Ta2 O6 1.995(3) 7_655 ? Ta2 O6 1.995(3) . ? Ta2 O5 2.001(3) . ? Ta2 O5 2.001(3) 7_655 ? Ta2 O1 2.3998(4) . ? O1 Ta1 2.3602(3) 5_665 ? O1 Ta1 2.3602(3) 7_655 ? O1 Ta1 2.3602(3) 3_565 ? O1 Ta2 2.3998(4) 5_665 ? O3 Ta1 1.985(2) 3_565 ? O4 Na3 2.470(3) 6_666 ? O4 Na5 2.554(9) 1_554 ? O6 Ta1 1.983(3) 3_565 ? O7 Ta1 1.987(2) 7_655 ? O7 Na5 2.549(10) 1_554 ? O7 Na5 2.549(10) 7_654 ? O12 Na5 2.510(10) 3_566 ? O12 H12A 0.82(2) . ? O12 H12B 0.84(2) . ? O13 Na2 2.368(4) 1_565 ? O13 Na5 2.904(10) 1_554 ? O13 H13A 0.84(2) . ? O13 H13B 0.84(2) . ? O14 O14 0.913(15) 3_566 ? O14 Na5 1.703(13) 2_664 ? O14 Na5 2.230(11) 4_646 ? O15 O15 1.010(19) 5_657 ? O15 Na5 1.555(10) 3_567 ? O15 Na5 1.555(10) 5_667 ? O15 Na5 2.219(12) 7_645 ? O15 Na5 2.219(12) 1_545 ? O15 Na2 2.512(12) 5_656 ? O15 Na2 2.585(12) 1_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 O11 Na1 O13 105.25(15) . . ? O11 Na1 O13 105.25(15) . 7_655 ? O13 Na1 O13 91.51(17) . 7_655 ? O11 Na1 O5 103.41(15) . 7_655 ? O13 Na1 O5 148.57(16) . 7_655 ? O13 Na1 O5 93.18(11) 7_655 7_655 ? O11 Na1 Na2 110.21(16) . 1_565 ? O13 Na1 Na2 45.79(8) . 1_565 ? O13 Na1 Na2 45.79(8) 7_655 1_565 ? O5 Na1 Na2 131.94(10) 7_655 1_565 ? O11 Na1 Ta1 137.13(11) . 7_655 ? O13 Na1 Ta1 117.59(13) . 7_655 ? O13 Na1 Ta1 76.21(10) 7_655 7_655 ? O5 Na1 Ta1 34.98(7) 7_655 7_655 ? Na2 Na1 Ta1 100.96(7) 1_565 7_655 ? O11 Na1 Ta1 137.13(11) . . ? O13 Na1 Ta1 76.21(10) . . ? O13 Na1 Ta1 117.59(13) 7_655 . ? O5 Na1 Ta1 74.10(9) 7_655 . ? Na2 Na1 Ta1 100.96(7) 1_565 . ? Ta1 Na1 Ta1 58.63(4) 7_655 . ? O11 Na1 Na5 151.18(18) . 7_654 ? O13 Na1 Na5 77.83(17) . 7_654 ? O13 Na1 Na5 45.99(17) 7_655 7_654 ? O5 Na1 Na5 83.28(15) 7_655 7_654 ? Na2 Na1 Na5 51.29(14) 1_565 7_654 ? Ta1 Na1 Na5 49.83(13) 7_655 7_654 ? Ta1 Na1 Na5 71.69(14) . 7_654 ? O11 Na1 Na5 151.17(18) . 1_554 ? O13 Na1 Na5 45.99(17) . 1_554 ? O13 Na1 Na5 77.83(17) 7_655 1_554 ? O5 Na1 Na5 105.03(17) 7_655 1_554 ? Na2 Na1 Na5 51.29(14) 1_565 1_554 ? Ta1 Na1 Na5 71.69(14) 7_655 1_554 ? Ta1 Na1 Na5 49.83(13) . 1_554 ? Na5 Na1 Na5 39.5(3) 7_654 1_554 ? O11 Na1 H13B 114.8(12) . . ? O13 Na1 H13B 18.9(8) . . ? O13 Na1 H13B 103.7(13) 7_655 . ? O5 Na1 H13B 131.6(8) 7_655 . ? Na2 Na1 H13B 60.0(12) 1_565 . ? Ta1 Na1 H13B 106.0(11) 7_655 . ? Ta1 Na1 H13B 57.8(7) . . ? Na5 Na1 H13B 77.4(14) 7_654 . ? Na5 Na1 H13B 39.1(14) 1_554 . ? O10 Na2 O12 84.06(15) . . ? O10 Na2 O12 84.06(15) . 7_655 ? O12 Na2 O12 85.3(2) . 7_655 ? O10 Na2 O13 87.96(14) . 7_645 ? O12 Na2 O13 171.60(18) . 7_645 ? O12 Na2 O13 91.27(12) 7_655 7_645 ? O10 Na2 O13 87.96(14) . 1_545 ? O12 Na2 O13 91.27(12) . 1_545 ? O12 Na2 O13 171.60(18) 7_655 1_545 ? O13 Na2 O13 91.05(18) 7_645 1_545 ? O10 Na2 O15 173.1(3) . 5_656 ? O12 Na2 O15 101.0(2) . 5_656 ? O12 Na2 O15 101.0(2) 7_655 5_656 ? O13 Na2 O15 87.18(19) 7_645 5_656 ? O13 Na2 O15 87.18(19) 1_545 5_656 ? O10 Na2 O15 164.2(3) . 1_554 ? O12 Na2 O15 84.3(2) . 1_554 ? O12 Na2 O15 84.3(2) 7_655 1_554 ? O13 Na2 O15 103.02(19) 7_645 1_554 ? O13 Na2 O15 103.02(19) 1_545 1_554 ? O15 Na2 O15 22.8(4) 5_656 1_554 ? O10 Na2 Na5 138.7(2) . 5_666 ? O12 Na2 Na5 91.9(2) . 5_666 ? O12 Na2 Na5 54.6(2) 7_655 5_666 ? O13 Na2 Na5 92.4(2) 7_645 5_666 ? O13 Na2 Na5 133.3(2) 1_545 5_666 ? O15 Na2 Na5 46.6(2) 5_656 5_666 ? O15 Na2 Na5 31.3(2) 1_554 5_666 ? O10 Na2 Na5 138.7(2) . 3_566 ? O12 Na2 Na5 54.6(2) . 3_566 ? O12 Na2 Na5 91.9(2) 7_655 3_566 ? O13 Na2 Na5 133.3(2) 7_645 3_566 ? O13 Na2 Na5 92.4(2) 1_545 3_566 ? O15 Na2 Na5 46.6(2) 5_656 3_566 ? O15 Na2 Na5 31.3(2) 1_554 3_566 ? Na5 Na2 Na5 53.6(4) 5_666 3_566 ? O10 Na2 Na5 148.06(19) . 7_644 ? O12 Na2 Na5 127.4(2) . 7_644 ? O12 Na2 Na5 92.2(2) 7_655 7_644 ? O13 Na2 Na5 60.36(19) 7_645 7_644 ? O13 Na2 Na5 96.0(2) 1_545 7_644 ? O15 Na2 Na5 28.18(19) 5_656 7_644 ? O15 Na2 Na5 43.3(2) 1_554 7_644 ? Na5 Na2 Na5 47.8(3) 5_666 7_644 ? Na5 Na2 Na5 73.0(3) 3_566 7_644 ? O10 Na2 Na5 148.06(19) . 1_544 ? O12 Na2 Na5 92.2(2) . 1_544 ? O12 Na2 Na5 127.4(2) 7_655 1_544 ? O13 Na2 Na5 96.0(2) 7_645 1_544 ? O13 Na2 Na5 60.36(19) 1_545 1_544 ? O15 Na2 Na5 28.18(19) 5_656 1_544 ? O15 Na2 Na5 43.3(2) 1_554 1_544 ? Na5 Na2 Na5 73.0(3) 5_666 1_544 ? Na5 Na2 Na5 47.8(3) 3_566 1_544 ? Na5 Na2 Na5 49.6(3) 7_644 1_544 ? O10 Na2 Na3 48.12(14) . . ? O12 Na2 Na3 52.32(12) . . ? O12 Na2 Na3 52.32(12) 7_655 . ? O13 Na2 Na3 119.81(11) 7_645 . ? O13 Na2 Na3 119.81(11) 1_545 . ? O15 Na2 Na3 138.8(2) 5_656 . ? O15 Na2 Na3 116.0(2) 1_554 . ? Na5 Na2 Na3 98.22(19) 5_666 . ? Na5 Na2 Na3 98.22(19) 3_566 . ? Na5 Na2 Na3 143.78(18) 7_644 . ? Na5 Na2 Na3 143.78(18) 1_544 . ? O10 Na3 O2 179.84(19) . . ? O10 Na3 O4 91.21(11) . 4_645 ? O2 Na3 O4 88.71(11) . 4_645 ? O10 Na3 O4 91.21(11) . 6_556 ? O2 Na3 O4 88.71(11) . 6_556 ? O4 Na3 O4 114.30(17) 4_645 6_556 ? O10 Na3 O12 76.20(13) . 7_655 ? O2 Na3 O12 103.93(13) . 7_655 ? O4 Na3 O12 157.76(13) 4_645 7_655 ? O4 Na3 O12 84.65(11) 6_556 7_655 ? O10 Na3 O12 76.20(13) . . ? O2 Na3 O12 103.93(13) . . ? O4 Na3 O12 84.65(11) 4_645 . ? O4 Na3 O12 157.76(13) 6_556 . ? O12 Na3 O12 74.65(17) 7_655 . ? O10 Na3 Na2 45.14(12) . . ? O2 Na3 Na2 135.02(14) . . ? O4 Na3 Na2 113.52(9) 4_645 . ? O4 Na3 Na2 113.52(9) 6_556 . ? O12 Na3 Na2 45.09(9) 7_655 . ? O12 Na3 Na2 45.09(9) . . ? O10 Na3 Ta2 152.63(15) . . ? O2 Na3 Ta2 27.53(10) . . ? O4 Na3 Ta2 103.33(9) 4_645 . ? O4 Na3 Ta2 103.33(9) 6_556 . ? O12 Na3 Ta2 82.13(10) 7_655 . ? O12 Na3 Ta2 82.13(10) . . ? Na2 Na3 Ta2 107.49(9) . . ? O10 Na3 Na4 141.32(14) . . ? O2 Na3 Na4 38.53(10) . . ? O4 Na3 Na4 69.19(9) 4_645 . ? O4 Na3 Na4 69.19(9) 6_556 . ? O12 Na3 Na4 131.33(9) 7_655 . ? O12 Na3 Na4 131.33(9) . . ? Na2 Na3 Na4 173.55(10) . . ? Ta2 Na3 Na4 66.06(4) . . ? O14 Na4 O14 156.6(4) . 7_655 ? O14 Na4 O14 180.0 . 5_666 ? O14 Na4 O14 23.4(4) 7_655 5_666 ? O14 Na4 O14 23.4(4) . 3_566 ? O14 Na4 O14 180.000(1) 7_655 3_566 ? O14 Na4 O14 156.6(4) 5_666 3_566 ? O14 Na4 O2 91.9(2) . 5_666 ? O14 Na4 O2 91.9(2) 7_655 5_666 ? O14 Na4 O2 88.1(2) 5_666 5_666 ? O14 Na4 O2 88.1(2) 3_566 5_666 ? O14 Na4 O11 78.41(18) . . ? O14 Na4 O11 78.41(18) 7_655 . ? O14 Na4 O11 101.59(18) 5_666 . ? O14 Na4 O11 101.59(18) 3_566 . ? O2 Na4 O11 90.64(14) 5_666 . ? O14 Na4 O11 101.59(18) . 5_666 ? O14 Na4 O11 101.59(18) 7_655 5_666 ? O14 Na4 O11 78.41(18) 5_666 5_666 ? O14 Na4 O11 78.41(18) 3_566 5_666 ? O2 Na4 O11 89.36(14) 5_666 5_666 ? O11 Na4 O11 180.0 . 5_666 ? O14 Na4 Na5 9.9(2) . 2_664 ? O14 Na4 Na5 150.0(2) 7_655 2_664 ? O14 Na4 Na5 170.1(2) 5_666 2_664 ? O14 Na4 Na5 30.0(2) 3_566 2_664 ? O2 Na4 Na5 84.59(14) 5_666 2_664 ? O11 Na4 Na5 71.87(13) . 2_664 ? O11 Na4 Na5 108.13(13) 5_666 2_664 ? O14 Na4 Na5 170.1(2) . 6_557 ? O14 Na4 Na5 30.0(2) 7_655 6_557 ? O14 Na4 Na5 9.9(2) 5_666 6_557 ? O14 Na4 Na5 150.0(2) 3_566 6_557 ? O2 Na4 Na5 95.41(14) 5_666 6_557 ? O11 Na4 Na5 108.13(13) . 6_557 ? O11 Na4 Na5 71.87(13) 5_666 6_557 ? Na5 Na4 Na5 180.0 2_664 6_557 ? O14 Na4 Na5 150.0(2) . 8_575 ? O14 Na4 Na5 9.9(2) 7_655 8_575 ? O14 Na4 Na5 30.0(2) 5_666 8_575 ? O14 Na4 Na5 170.1(2) 3_566 8_575 ? O2 Na4 Na5 84.59(14) 5_666 8_575 ? O11 Na4 Na5 71.87(13) . 8_575 ? O11 Na4 Na5 108.13(13) 5_666 8_575 ? Na5 Na4 Na5 141.9(3) 2_664 8_575 ? Na5 Na4 Na5 38.1(3) 6_557 8_575 ? O14 Na4 Na5 30.0(2) . 4_646 ? O14 Na4 Na5 170.1(2) 7_655 4_646 ? O14 Na4 Na5 150.0(2) 5_666 4_646 ? O14 Na4 Na5 9.9(2) 3_566 4_646 ? O2 Na4 Na5 95.41(14) 5_666 4_646 ? O11 Na4 Na5 108.13(13) . 4_646 ? O11 Na4 Na5 71.87(13) 5_666 4_646 ? Na5 Na4 Na5 38.1(3) 2_664 4_646 ? Na5 Na4 Na5 141.9(3) 6_557 4_646 ? Na5 Na4 Na5 180.0(3) 8_575 4_646 ? O14 Na4 Na3 84.5(2) . 5_666 ? O14 Na4 Na3 84.5(2) 7_655 5_666 ? O14 Na4 Na3 95.5(2) 5_666 5_666 ? O14 Na4 Na3 95.5(2) 3_566 5_666 ? O2 Na4 Na3 37.37(11) 5_666 5_666 ? O11 Na4 Na3 53.27(11) . 5_666 ? O11 Na4 Na3 126.73(11) 5_666 5_666 ? Na5 Na4 Na3 74.66(13) 2_664 5_666 ? Na5 Na4 Na3 105.34(13) 6_557 5_666 ? Na5 Na4 Na3 74.66(13) 8_575 5_666 ? Na5 Na4 Na3 105.34(13) 4_646 5_666 ? O15 Na5 O14 120.3(7) 5_667 2_665 ? O15 Na5 O15 23.6(5) 5_667 1_565 ? O14 Na5 O15 96.9(5) 2_665 1_565 ? O15 Na5 O14 101.1(6) 5_667 4_656 ? O14 Na5 O14 22.1(4) 2_665 4_656 ? O15 Na5 O14 78.9(4) 1_565 4_656 ? O15 Na5 O12 106.0(6) 5_667 3_566 ? O14 Na5 O12 87.5(5) 2_665 3_566 ? O15 Na5 O12 104.0(5) 1_565 3_566 ? O14 Na5 O12 104.1(4) 4_656 3_566 ? O15 Na5 Na5 60.5(5) 5_667 3_577 ? O14 Na5 Na5 60.0(4) 2_665 3_577 ? O15 Na5 Na5 37.6(3) 1_565 3_577 ? O14 Na5 Na5 41.4(3) 4_656 3_577 ? O12 Na5 Na5 106.7(5) 3_566 3_577 ? O15 Na5 O7 84.4(5) 5_667 1_556 ? O14 Na5 O7 152.0(5) 2_665 1_556 ? O15 Na5 O7 107.9(4) 1_565 1_556 ? O14 Na5 O7 153.9(5) 4_656 1_556 ? O12 Na5 O7 98.7(3) 3_566 1_556 ? Na5 Na5 O7 140.9(4) 3_577 1_556 ? O15 Na5 O4 149.1(7) 5_667 1_556 ? O14 Na5 O4 81.8(4) 2_665 1_556 ? O15 Na5 O4 160.4(5) 1_565 1_556 ? O14 Na5 O4 94.6(4) 4_656 1_556 ? O12 Na5 O4 95.5(3) 3_566 1_556 ? Na5 Na5 O4 133.8(3) 3_577 1_556 ? O7 Na5 O4 70.5(2) 1_556 1_556 ? O15 Na5 Na5 29.8(5) 5_667 7_655 ? O14 Na5 Na5 149.1(4) 2_665 7_655 ? O15 Na5 Na5 52.5(3) 1_565 7_655 ? O14 Na5 Na5 130.9(3) 4_656 7_655 ? O12 Na5 Na5 95.1(2) 3_566 7_655 ? Na5 Na5 Na5 90.000(3) 3_577 7_655 ? O7 Na5 Na5 58.0(2) 1_556 7_655 ? O4 Na5 Na5 128.4(2) 1_556 7_655 ? O15 Na5 O13 93.0(6) 5_667 1_556 ? O14 Na5 O13 91.6(4) 2_665 1_556 ? O15 Na5 O13 97.5(4) 1_565 1_556 ? O14 Na5 O13 81.5(3) 4_656 1_556 ? O12 Na5 O13 158.4(4) 3_566 1_556 ? Na5 Na5 O13 91.3(5) 3_577 1_556 ? O7 Na5 O13 72.8(3) 1_556 1_556 ? O4 Na5 O13 63.0(2) 1_556 1_556 ? Na5 Na5 O13 96.7(2) 7_655 1_556 ? O15 Na5 Na2 59.8(5) 5_667 5_666 ? O14 Na5 Na2 97.2(4) 2_665 5_666 ? O15 Na5 Na2 55.3(4) 1_565 5_666 ? O14 Na5 Na2 97.1(4) 4_656 5_666 ? O12 Na5 Na2 48.93(18) 3_566 5_666 ? Na5 Na5 Na2 70.8(3) 3_577 5_666 ? O7 Na5 Na2 107.5(3) 1_556 5_666 ? O4 Na5 Na2 144.4(4) 1_556 5_666 ? Na5 Na5 Na2 63.18(18) 7_655 5_666 ? O13 Na5 Na2 152.1(3) 1_556 5_666 ? O15 Na5 Ta1 123.2(6) 5_667 1_556 ? O14 Na5 Ta1 115.2(5) 2_665 1_556 ? O15 Na5 Ta1 146.7(4) 1_565 1_556 ? O14 Na5 Ta1 129.5(4) 4_656 1_556 ? O12 Na5 Ta1 87.0(3) 3_566 1_556 ? Na5 Na5 Ta1 164.6(5) 3_577 1_556 ? O7 Na5 Ta1 38.85(14) 1_556 1_556 ? O4 Na5 Ta1 34.88(13) 1_556 1_556 ? Na5 Na5 Ta1 95.79(17) 7_655 1_556 ? O13 Na5 Ta1 73.9(2) 1_556 1_556 ? Na2 Na5 Ta1 124.5(3) 5_666 1_556 ? O4 Ta1 O6 103.05(13) . 3_565 ? O4 Ta1 O3 102.78(14) . . ? O6 Ta1 O3 86.70(8) 3_565 . ? O4 Ta1 O7 101.57(14) . . ? O6 Ta1 O7 87.71(15) 3_565 . ? O3 Ta1 O7 155.65(13) . . ? O4 Ta1 O5 101.13(13) . . ? O6 Ta1 O5 155.81(11) 3_565 . ? O3 Ta1 O5 88.47(8) . . ? O7 Ta1 O5 86.98(15) . . ? O4 Ta1 O1 178.99(10) . . ? O6 Ta1 O1 77.78(8) 3_565 . ? O3 Ta1 O1 77.80(9) . . ? O7 Ta1 O1 77.85(10) . . ? O5 Ta1 O1 78.03(8) . . ? O4 Ta1 Na5 53.8(2) . 1_554 ? O6 Ta1 Na5 78.21(18) 3_565 1_554 ? O3 Ta1 Na5 146.99(19) . 1_554 ? O7 Ta1 Na5 53.6(2) . 1_554 ? O5 Ta1 Na5 116.60(18) . 1_554 ? O1 Ta1 Na5 126.03(17) . 1_554 ? O4 Ta1 Ta1 135.57(10) . 3_565 ? O6 Ta1 Ta1 80.86(8) 3_565 3_565 ? O3 Ta1 Ta1 32.80(9) . 3_565 ? O7 Ta1 Ta1 122.85(10) . 3_565 ? O5 Ta1 Ta1 82.29(8) . 3_565 ? O1 Ta1 Ta1 45.002(8) . 3_565 ? Na5 Ta1 Ta1 158.86(16) 1_554 3_565 ? O4 Ta1 Ta1 134.41(10) . 7_655 ? O6 Ta1 Ta1 81.93(8) 3_565 7_655 ? O3 Ta1 Ta1 122.80(9) . 7_655 ? O7 Ta1 Ta1 32.86(10) . 7_655 ? O5 Ta1 Ta1 80.85(8) . 7_655 ? O1 Ta1 Ta1 44.998(8) . 7_655 ? Na5 Ta1 Ta1 84.21(17) 1_554 7_655 ? Ta1 Ta1 Ta1 90.0 3_565 7_655 ? O4 Ta1 Na1 88.78(10) . . ? O6 Ta1 Na1 135.34(9) 3_565 . ? O3 Ta1 Na1 132.95(4) . . ? O7 Ta1 Na1 47.63(12) . . ? O5 Ta1 Na1 44.48(9) . . ? O1 Ta1 Na1 90.22(3) . . ? Na5 Ta1 Na1 74.78(17) 1_554 . ? Ta1 Ta1 Na1 119.67(4) 3_565 . ? Ta1 Ta1 Na1 60.68(2) 7_655 . ? O2 Ta2 O6 101.09(13) . 7_655 ? O2 Ta2 O6 101.09(13) . . ? O6 Ta2 O6 88.36(16) 7_655 . ? O2 Ta2 O5 105.51(13) . . ? O6 Ta2 O5 153.39(11) 7_655 . ? O6 Ta2 O5 87.22(12) . . ? O2 Ta2 O5 105.51(13) . 7_655 ? O6 Ta2 O5 87.22(12) 7_655 7_655 ? O6 Ta2 O5 153.39(11) . 7_655 ? O5 Ta2 O5 85.09(16) . 7_655 ? O2 Ta2 O1 176.72(14) . . ? O6 Ta2 O1 76.61(8) 7_655 . ? O6 Ta2 O1 76.61(8) . . ? O5 Ta2 O1 76.84(8) . . ? O5 Ta2 O1 76.84(8) 7_655 . ? O2 Ta2 Na3 38.94(14) . . ? O6 Ta2 Na3 73.47(9) 7_655 . ? O6 Ta2 Na3 73.47(9) . . ? O5 Ta2 Na3 129.75(8) . . ? O5 Ta2 Na3 129.75(8) 7_655 . ? O1 Ta2 Na3 137.78(4) . . ? Ta1 O1 Ta1 180.0 . 5_665 ? Ta1 O1 Ta1 90.004(15) . 7_655 ? Ta1 O1 Ta1 89.996(15) 5_665 7_655 ? Ta1 O1 Ta1 89.996(15) . 3_565 ? Ta1 O1 Ta1 90.004(15) 5_665 3_565 ? Ta1 O1 Ta1 180.0 7_655 3_565 ? Ta1 O1 Ta2 90.009(7) . 5_665 ? Ta1 O1 Ta2 89.991(7) 5_665 5_665 ? Ta1 O1 Ta2 90.009(7) 7_655 5_665 ? Ta1 O1 Ta2 89.991(7) 3_565 5_665 ? Ta1 O1 Ta2 89.991(7) . . ? Ta1 O1 Ta2 90.009(6) 5_665 . ? Ta1 O1 Ta2 89.991(7) 7_655 . ? Ta1 O1 Ta2 90.009(6) 3_565 . ? Ta2 O1 Ta2 180.000(10) 5_665 . ? Ta2 O2 Na3 113.5(2) . . ? Ta1 O3 Ta1 114.40(18) 3_565 . ? Ta1 O4 Na3 127.05(16) . 6_666 ? Ta1 O4 Na5 91.3(2) . 1_554 ? Na3 O4 Na5 138.9(2) 6_666 1_554 ? Ta1 O5 Ta2 115.11(13) . . ? Ta1 O6 Ta2 115.59(13) 3_565 . ? Ta1 O7 Ta1 114.3(2) 7_655 . ? Ta1 O7 Na5 147.9(3) 7_655 1_554 ? Ta1 O7 Na5 87.6(2) . 1_554 ? Ta1 O7 Na5 87.6(2) 7_655 7_654 ? Ta1 O7 Na5 147.9(3) . 7_654 ? Na5 O7 Na5 64.0(4) 1_554 7_654 ? Na2 O10 Na3 86.74(18) . . ? Na1 O11 Na4 123.2(2) . . ? Na2 O12 Na5 76.4(2) . 3_566 ? Na2 O12 Na3 82.58(13) . . ? Na5 O12 Na3 135.3(3) 3_566 . ? Na2 O12 H12A 138(4) . . ? Na5 O12 H12A 77(5) 3_566 . ? Na3 O12 H12A 95(5) . . ? Na2 O12 H12B 114(4) . . ? Na5 O12 H12B 127(5) 3_566 . ? Na3 O12 H12B 97(5) . . ? H12A O12 H12B 107(3) . . ? Na1 O13 Na2 88.65(12) . 1_565 ? Na1 O13 Na5 98.3(2) . 1_554 ? Na2 O13 Na5 74.5(2) 1_565 1_554 ? Na1 O13 H13A 121(5) . . ? Na2 O13 H13A 112(4) 1_565 . ? Na5 O13 H13A 140(5) 1_554 . ? Na1 O13 H13B 95(5) . . ? Na2 O13 H13B 133(5) 1_565 . ? Na5 O13 H13B 59(5) 1_554 . ? H13A O13 H13B 106(3) . . ? O14 O14 Na5 113.5(5) 3_566 2_664 ? O14 O14 Na5 44.4(5) 3_566 4_646 ? Na5 O14 Na5 78.7(6) 2_664 4_646 ? O14 O14 Na4 78.28(18) 3_566 . ? Na5 O14 Na4 157.0(5) 2_664 . ? Na5 O14 Na4 119.7(4) 4_646 . ? O15 O15 Na5 118.3(5) 5_657 3_567 ? O15 O15 Na5 118.3(5) 5_657 5_667 ? Na5 O15 Na5 120.4(9) 3_567 5_667 ? O15 O15 Na5 38.1(3) 5_657 7_645 ? Na5 O15 Na5 156.4(5) 3_567 7_645 ? Na5 O15 Na5 82.0(6) 5_667 7_645 ? O15 O15 Na5 38.1(3) 5_657 1_545 ? Na5 O15 Na5 82.0(6) 3_567 1_545 ? Na5 O15 Na5 156.4(5) 5_667 1_545 ? Na5 O15 Na5 74.9(6) 7_645 1_545 ? O15 O15 Na2 82.7(13) 5_657 5_656 ? Na5 O15 Na2 102.1(6) 3_567 5_656 ? Na5 O15 Na2 102.1(6) 5_667 5_656 ? Na5 O15 Na2 78.2(4) 7_645 5_656 ? Na5 O15 Na2 78.2(4) 1_545 5_656 ? O15 O15 Na2 74.5(13) 5_657 1_556 ? Na5 O15 Na2 88.9(6) 3_567 1_556 ? Na5 O15 Na2 88.9(6) 5_667 1_556 ? Na5 O15 Na2 83.8(4) 7_645 1_556 ? Na5 O15 Na2 83.8(4) 1_545 1_556 ? Na2 O15 Na2 157.2(4) 5_656 1_556 ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 2.143 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.257 # start Validation Reply Form _vrf_PLAT306_na8ta6 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O10 RESPONSE: ...Not all hydrogen atoms could be located for water molecules in the structure. However, proper hydrogen content (assuming all isolated oxygen atoms are water molecules) was added to the composition during the final refinement to obtain proper calculated crystal data. ; # end Validation Reply Form