data_huemm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H48 Al Mg Na4 O52 V10' _chemical_formula_weight 1533.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 '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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.668(4) _cell_length_b 10.295(4) _cell_length_c 12.908(5) _cell_angle_alpha 105.826(9) _cell_angle_beta 97.899(9) _cell_angle_gamma 103.385(9) _cell_volume 1053.0(8) _cell_formula_units_Z 1 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 763 _exptl_absorpt_coefficient_mu 2.334 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16578 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0858 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.44 _reflns_number_total 5234 _reflns_number_gt 3244 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0412P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5234 _refine_ls_number_parameters 384 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 10.368 _refine_ls_shift/su_mean 0.027 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 V1 V 0.19664(7) 0.07252(7) 0.53427(5) 0.01258(16) Uani 1 1 d . . . V2 V 0.00684(8) -0.01910(7) 0.70657(5) 0.01403(17) Uani 1 1 d . . . V3 V 0.05702(8) -0.24605(7) 0.51040(5) 0.01305(17) Uani 1 1 d . . . V4 V 0.13793(8) 0.29976(7) 0.72602(6) 0.01593(18) Uani 1 1 d . . . V5 V 0.23092(8) -0.15303(7) 0.33568(6) 0.01550(18) Uani 1 1 d . . . O1 O 0.0777(3) -0.3380(3) 0.5906(2) 0.0206(7) Uani 1 1 d . . . O2 O 0.0306(3) -0.1114(3) 0.7861(2) 0.0219(7) Uani 1 1 d . . . O3 O 0.2935(3) 0.2256(3) 0.6399(2) 0.0152(6) Uani 1 1 d . . . O4 O 0.1426(3) 0.1546(3) 0.7872(2) 0.0161(6) Uani 1 1 d . . . O5 O 0.0639(3) -0.3000(3) 0.2426(2) 0.0165(6) Uani 1 1 d . . . O6 O 0.3388(3) 0.0267(3) 0.4679(2) 0.0163(6) Uani 1 1 d . . . O7 O 0.1205(3) 0.1691(3) 0.4334(2) 0.0116(6) Uani 1 1 d . . . O8 O 0.3853(3) -0.1811(3) 0.2887(2) 0.0240(7) Uani 1 1 d . . . O9 O 0.1756(3) -0.0537(3) 0.6175(2) 0.0119(6) Uani 1 1 d . . . O10 O 0.2318(3) -0.2436(3) 0.4451(2) 0.0155(6) Uani 1 1 d . . . O11 O -0.0937(3) -0.3713(3) 0.3912(2) 0.0154(6) Uani 1 1 d . . . O12 O -0.1796(3) 0.0251(3) 0.7324(2) 0.0165(6) Uani 1 1 d . . . O13 O 0.0236(3) -0.0972(3) 0.4164(2) 0.0124(6) Uani 1 1 d . . . O14 O 0.2603(3) 0.4354(3) 0.8177(2) 0.0273(7) Uani 1 1 d . . . Al1 Al 0.5000 0.5000 0.5000 0.0138(6) Uani 0.993(7) 2 d SP . . Na1 Na 0.5000 0.0000 1.0000 0.0458(12) Uani 1.027(10) 2 d SP . . Na2 Na 0.0840(2) -0.23409(19) 0.91567(14) 0.0309(7) Uani 1.002(6) 1 d P . . O15 O 0.3401(6) -0.2340(5) 0.8678(4) 0.0477(11) Uani 1 1 d . . . O16 O -0.1577(5) -0.2284(4) 0.9817(3) 0.0361(9) Uani 1 1 d . . . O17 O 0.2394(5) -0.0098(4) 1.0568(3) 0.0344(9) Uani 1 1 d . . . O18 O 0.1335(6) -0.3768(5) 1.0298(3) 0.0425(10) Uani 1 1 d D . . O19 O 0.3240(4) 0.3649(4) 0.3938(3) 0.0219(7) Uani 1 1 d . . . O20 O 0.3641(4) 0.5526(4) 0.5967(3) 0.0225(8) Uani 1 1 d . . . O21 O 0.4653(4) 0.6348(3) 0.4336(3) 0.0222(7) Uani 1 1 d . . . O22 O -0.0907(5) -0.4258(4) 0.7443(3) 0.0314(9) Uani 1 1 d . . . O23 O 0.4448(6) 0.1295(6) 0.8839(4) 0.0550(14) Uani 1 1 d . . . O24 O 0.3910(6) -0.4946(6) 1.0844(5) 0.0970(18) Uani 1 1 d . . . O25 O 0.4448(6) 0.8361(4) 0.6853(3) 0.0340(10) Uani 1 1 d . . . H15A H 0.365(9) -0.234(8) 0.816(6) 0.09(3) Uiso 1 1 d . . . H15B H 0.395(11) -0.276(10) 0.891(7) 0.15(5) Uiso 1 1 d . . . H16A H -0.229(6) -0.292(5) 0.954(4) 0.021(15) Uiso 1 1 d . . . H16B H -0.147(5) -0.209(5) 1.048(4) 0.025(14) Uiso 1 1 d . . . H17A H 0.222(6) -0.007(5) 1.119(4) 0.038(16) Uiso 1 1 d . . . H17B H 0.209(6) 0.053(5) 1.054(4) 0.021(16) Uiso 1 1 d . . . H18A H 0.117(8) -0.347(7) 1.085(5) 0.06(2) Uiso 1 1 d . . . H18B H 0.209(6) -0.411(7) 1.042(6) 0.12(4) Uiso 1 1 d D . . H19A H 0.264(6) 0.308(6) 0.404(4) 0.041(18) Uiso 1 1 d . . . H19B H 0.269(5) 0.394(4) 0.353(3) 0.004(11) Uiso 1 1 d . . . H20A H 0.289(5) 0.514(5) 0.590(3) 0.011(13) Uiso 1 1 d . . . H20B H 0.385(6) 0.646(6) 0.638(4) 0.051(17) Uiso 1 1 d . . . H21A H 0.531(6) 0.672(5) 0.408(4) 0.028(14) Uiso 1 1 d . . . H21B H 0.385(6) 0.667(5) 0.433(4) 0.029(14) Uiso 1 1 d . . . H22A H -0.093(6) -0.486(5) 0.754(4) 0.021(17) Uiso 1 1 d . . . H22B H 0.018(11) -0.409(9) 0.693(7) 0.18(4) Uiso 1 1 d . . . H23A H 0.369(7) 0.140(7) 0.851(5) 0.07(3) Uiso 1 1 d . . . H23B H 0.492(6) 0.131(5) 0.848(4) 0.022(17) Uiso 1 1 d . . . H24A H 0.443(7) -0.413(6) 1.054(5) 0.064(19) Uiso 1 1 d . . . H24B H 0.414(7) -0.554(6) 1.160(5) 0.08(2) Uiso 1 1 d . . . H25A H 0.544(8) 0.873(7) 0.690(5) 0.08(2) Uiso 1 1 d . . . H25B H 0.404(7) 0.877(6) 0.675(5) 0.04(2) 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 V1 0.0099(3) 0.0133(4) 0.0161(4) 0.0073(3) 0.0031(3) 0.0030(3) V2 0.0186(4) 0.0142(4) 0.0123(4) 0.0073(3) 0.0045(3) 0.0059(3) V3 0.0148(3) 0.0124(4) 0.0162(4) 0.0082(3) 0.0056(3) 0.0062(3) V4 0.0174(4) 0.0142(4) 0.0158(4) 0.0040(3) 0.0035(3) 0.0045(3) V5 0.0151(3) 0.0183(4) 0.0178(4) 0.0085(3) 0.0078(3) 0.0077(3) O1 0.0233(15) 0.0213(17) 0.0246(17) 0.0146(14) 0.0085(13) 0.0095(13) O2 0.0308(16) 0.0203(17) 0.0225(17) 0.0143(14) 0.0098(13) 0.0108(14) O3 0.0118(13) 0.0154(15) 0.0192(15) 0.0082(12) 0.0027(11) 0.0023(12) O4 0.0200(14) 0.0140(15) 0.0148(15) 0.0052(12) 0.0032(12) 0.0056(12) O5 0.0219(14) 0.0147(15) 0.0155(15) 0.0055(12) 0.0059(12) 0.0081(12) O6 0.0110(13) 0.0189(16) 0.0209(15) 0.0079(13) 0.0048(11) 0.0048(12) O7 0.0129(13) 0.0102(14) 0.0138(14) 0.0058(11) 0.0051(11) 0.0033(11) O8 0.0255(16) 0.0300(18) 0.0262(17) 0.0147(14) 0.0127(13) 0.0153(14) O9 0.0133(13) 0.0112(14) 0.0136(14) 0.0077(11) 0.0016(11) 0.0039(11) O10 0.0179(14) 0.0160(15) 0.0175(15) 0.0078(12) 0.0072(12) 0.0088(12) O11 0.0145(13) 0.0140(15) 0.0193(15) 0.0065(12) 0.0048(11) 0.0051(12) O12 0.0179(14) 0.0197(16) 0.0170(15) 0.0111(13) 0.0073(12) 0.0067(12) O13 0.0093(12) 0.0157(15) 0.0150(14) 0.0091(12) 0.0032(11) 0.0036(11) O14 0.0273(17) 0.0224(17) 0.0262(18) 0.0036(14) 0.0019(14) 0.0024(14) Al1 0.0117(9) 0.0118(10) 0.0217(11) 0.0094(8) 0.0064(7) 0.0039(7) Na1 0.0314(16) 0.066(2) 0.043(2) 0.0248(16) 0.0088(13) 0.0102(15) Na2 0.0360(11) 0.0330(13) 0.0271(11) 0.0150(9) 0.0067(8) 0.0101(9) O15 0.054(3) 0.055(3) 0.044(3) 0.019(2) 0.021(2) 0.024(2) O16 0.045(2) 0.040(3) 0.021(2) 0.0070(19) 0.0111(18) 0.010(2) O17 0.045(2) 0.039(2) 0.029(2) 0.0151(19) 0.0177(18) 0.021(2) O18 0.061(3) 0.050(3) 0.028(2) 0.017(2) 0.015(2) 0.030(2) O19 0.0164(15) 0.0201(19) 0.0299(19) 0.0157(15) 0.0013(14) -0.0008(14) O20 0.0153(16) 0.0184(19) 0.034(2) 0.0079(16) 0.0124(15) 0.0004(15) O21 0.0188(16) 0.0205(18) 0.038(2) 0.0216(16) 0.0127(15) 0.0082(15) O22 0.041(2) 0.024(2) 0.037(2) 0.0185(18) 0.0119(16) 0.0110(18) O23 0.037(2) 0.103(4) 0.051(3) 0.048(3) 0.020(2) 0.035(3) O24 0.057(3) 0.077(4) 0.148(6) 0.041(4) -0.004(3) 0.010(3) O25 0.032(2) 0.028(2) 0.041(2) 0.0110(19) 0.0054(18) 0.008(2) _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 V1 O6 1.677(3) . ? V1 O3 1.717(3) . ? V1 O9 1.893(3) . ? V1 O7 1.972(3) . ? V1 O13 2.080(3) . ? V1 O13 2.141(3) 2_556 ? V1 V5 3.0550(13) . ? V1 V4 3.0979(13) . ? V2 O2 1.602(3) . ? V2 O12 1.827(3) . ? V2 O4 1.828(3) . ? V2 O7 2.002(3) 2_556 ? V2 O9 2.017(3) . ? V2 O13 2.256(3) 2_556 ? V2 V5 3.0974(13) 2_556 ? V2 V3 3.0993(13) . ? V3 O1 1.601(3) . ? V3 O11 1.822(3) . ? V3 O10 1.830(3) . ? V3 O9 2.015(3) . ? V3 O7 2.020(3) 2_556 ? V3 O13 2.242(3) . ? V3 V4 3.1150(15) 2_556 ? V3 V5 3.1175(13) . ? V4 O14 1.595(3) . ? V4 O5 1.850(3) 2_556 ? V4 O4 1.876(3) . ? V4 O11 1.887(3) 2_556 ? V4 O3 2.016(3) . ? V4 O13 2.354(3) 2_556 ? V4 V5 3.0896(16) 2_556 ? V4 V3 3.1150(15) 2_556 ? V5 O8 1.597(3) . ? V5 O5 1.828(3) . ? V5 O12 1.871(3) 2_556 ? V5 O10 1.893(3) . ? V5 O6 2.061(3) . ? V5 O13 2.305(3) . ? V5 V4 3.0896(16) 2_556 ? V5 V2 3.0974(13) 2_556 ? O2 Na2 2.411(3) . ? O5 V4 1.850(3) 2_556 ? O7 V2 2.002(3) 2_556 ? O7 V3 2.020(3) 2_556 ? O11 V4 1.887(3) 2_556 ? O12 V5 1.871(3) 2_556 ? O13 V1 2.141(3) 2_556 ? O13 V2 2.256(3) 2_556 ? O13 V4 2.354(3) 2_556 ? Al1 O21 1.876(3) . ? Al1 O21 1.876(3) 2_666 ? Al1 O19 1.882(3) . ? Al1 O19 1.882(3) 2_666 ? Al1 O20 1.889(3) . ? Al1 O20 1.889(3) 2_666 ? Na1 O23 2.332(5) 2_657 ? Na1 O23 2.332(5) . ? Na1 O17 2.458(4) 2_657 ? Na1 O17 2.458(4) . ? Na1 O15 2.489(5) 2_657 ? Na1 O15 2.489(5) . ? Na1 Na2 3.669(2) . ? Na1 Na2 3.669(2) 2_657 ? Na2 O16 2.375(4) . ? Na2 O15 2.384(5) . ? Na2 O18 2.410(4) . ? Na2 O17 2.461(4) . ? Na2 O22 2.529(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 V1 O3 106.62(13) . . ? O6 V1 O9 99.98(12) . . ? O3 V1 O9 98.61(12) . . ? O6 V1 O7 95.47(12) . . ? O3 V1 O7 94.25(12) . . ? O9 V1 O7 156.12(11) . . ? O6 V1 O13 88.50(12) . . ? O3 V1 O13 164.41(12) . . ? O9 V1 O13 82.09(11) . . ? O7 V1 O13 80.21(11) . . ? O6 V1 O13 166.31(12) . 2_556 ? O3 V1 O13 86.45(11) . 2_556 ? O9 V1 O13 81.66(10) . 2_556 ? O7 V1 O13 79.14(10) . 2_556 ? O13 V1 O13 78.22(11) . 2_556 ? O6 V1 V5 39.58(9) . . ? O3 V1 V5 146.15(9) . . ? O9 V1 V5 91.33(9) . . ? O7 V1 V5 89.05(8) . . ? O13 V1 V5 48.95(7) . . ? O13 V1 V5 127.14(7) 2_556 . ? O6 V1 V4 143.71(10) . . ? O3 V1 V4 37.13(9) . . ? O9 V1 V4 90.14(9) . . ? O7 V1 V4 88.05(8) . . ? O13 V1 V4 127.57(8) . . ? O13 V1 V4 49.35(7) 2_556 . ? V5 V1 V4 175.90(3) . . ? O2 V2 O12 102.27(13) . . ? O2 V2 O4 102.66(14) . . ? O12 V2 O4 95.34(13) . . ? O2 V2 O7 101.04(13) . 2_556 ? O12 V2 O7 89.52(11) . 2_556 ? O4 V2 O7 154.16(11) . 2_556 ? O2 V2 O9 100.24(13) . . ? O12 V2 O9 155.20(11) . . ? O4 V2 O9 89.72(11) . . ? O7 V2 O9 76.03(11) 2_556 . ? O2 V2 O13 175.42(13) . 2_556 ? O12 V2 O13 80.72(10) . 2_556 ? O4 V2 O13 80.37(11) . 2_556 ? O7 V2 O13 75.39(10) 2_556 2_556 ? O9 V2 O13 76.22(10) . 2_556 ? O2 V2 V5 135.48(11) . 2_556 ? O12 V2 V5 33.55(8) . 2_556 ? O4 V2 V5 82.98(9) . 2_556 ? O7 V2 V5 87.32(8) 2_556 2_556 ? O9 V2 V5 124.10(8) . 2_556 ? O13 V2 V5 47.89(7) 2_556 2_556 ? O2 V2 V3 90.87(11) . . ? O12 V2 V3 129.32(9) . . ? O4 V2 V3 129.45(9) . . ? O7 V2 V3 39.80(8) 2_556 . ? O9 V2 V3 39.74(7) . . ? O13 V2 V3 84.55(8) 2_556 . ? V5 V2 V3 119.71(4) 2_556 . ? O1 V3 O11 102.85(14) . . ? O1 V3 O10 104.09(13) . . ? O11 V3 O10 96.40(12) . . ? O1 V3 O9 98.87(13) . . ? O11 V3 O9 155.21(12) . . ? O10 V3 O9 89.72(11) . . ? O1 V3 O7 98.55(12) . 2_556 ? O11 V3 O7 89.29(11) . 2_556 ? O10 V3 O7 154.72(11) . 2_556 ? O9 V3 O7 75.69(11) . 2_556 ? O1 V3 O13 172.75(12) . . ? O11 V3 O13 81.82(11) . . ? O10 V3 O13 80.66(10) . . ? O9 V3 O13 75.49(10) . . ? O7 V3 O13 75.79(10) 2_556 . ? O1 V3 V2 88.45(11) . . ? O11 V3 V2 128.68(9) . . ? O10 V3 V2 129.50(9) . . ? O9 V3 V2 39.79(7) . . ? O7 V3 V2 39.39(7) 2_556 . ? O13 V3 V2 84.31(8) . . ? O1 V3 V4 136.28(11) . 2_556 ? O11 V3 V4 33.53(8) . 2_556 ? O10 V3 V4 84.61(9) . 2_556 ? O9 V3 V4 124.27(8) . 2_556 ? O7 V3 V4 86.77(8) 2_556 2_556 ? O13 V3 V4 48.86(7) . 2_556 ? V2 V3 V4 119.09(4) . 2_556 ? O1 V3 V5 137.72(10) . . ? O11 V3 V5 84.68(9) . . ? O10 V3 V5 33.78(8) . . ? O9 V3 V5 87.28(8) . . ? O7 V3 V5 123.33(8) 2_556 . ? O13 V3 V5 47.56(7) . . ? V2 V3 V5 119.32(4) . . ? V4 V3 V5 59.43(4) 2_556 . ? O14 V4 O5 104.48(14) . 2_556 ? O14 V4 O4 103.45(14) . . ? O5 V4 O4 90.14(12) 2_556 . ? O14 V4 O11 101.59(14) . 2_556 ? O5 V4 O11 91.05(12) 2_556 2_556 ? O4 V4 O11 153.79(12) . 2_556 ? O14 V4 O3 100.55(14) . . ? O5 V4 O3 154.97(12) 2_556 . ? O4 V4 O3 84.49(11) . . ? O11 V4 O3 83.43(11) 2_556 . ? O14 V4 O13 175.07(13) . 2_556 ? O5 V4 O13 80.42(10) 2_556 2_556 ? O4 V4 O13 76.85(11) . 2_556 ? O11 V4 O13 77.54(11) 2_556 2_556 ? O3 V4 O13 74.55(10) . 2_556 ? O14 V4 V5 137.12(11) . 2_556 ? O5 V4 V5 32.64(8) 2_556 2_556 ? O4 V4 V5 82.49(9) . 2_556 ? O11 V4 V5 84.49(8) 2_556 2_556 ? O3 V4 V5 122.33(8) . 2_556 ? O13 V4 V5 47.78(6) 2_556 2_556 ? O14 V4 V1 131.46(12) . . ? O5 V4 V1 124.05(9) 2_556 . ? O4 V4 V1 77.94(9) . . ? O11 V4 V1 79.75(9) 2_556 . ? O3 V4 V1 30.93(7) . . ? O13 V4 V1 43.65(7) 2_556 . ? V5 V4 V1 91.41(3) 2_556 . ? O14 V4 V3 133.72(12) . 2_556 ? O5 V4 V3 80.81(9) 2_556 2_556 ? O4 V4 V3 122.67(9) . 2_556 ? O11 V4 V3 32.24(8) 2_556 2_556 ? O3 V4 V3 81.62(8) . 2_556 ? O13 V4 V3 45.84(7) 2_556 2_556 ? V5 V4 V3 60.32(3) 2_556 2_556 ? V1 V4 V3 62.51(3) . 2_556 ? O8 V5 O5 102.76(14) . . ? O8 V5 O12 101.73(13) . 2_556 ? O5 V5 O12 93.12(12) . 2_556 ? O8 V5 O10 101.24(13) . . ? O5 V5 O10 90.78(12) . . ? O12 V5 O10 155.21(12) 2_556 . ? O8 V5 O6 100.94(13) . . ? O5 V5 O6 156.29(11) . . ? O12 V5 O6 82.95(12) 2_556 . ? O10 V5 O6 83.68(11) . . ? O8 V5 O13 174.98(13) . . ? O5 V5 O13 82.20(11) . . ? O12 V5 O13 78.54(10) 2_556 . ? O10 V5 O13 77.76(10) . . ? O6 V5 O13 74.09(10) . . ? O8 V5 V1 132.14(11) . . ? O5 V5 V1 125.05(9) . . ? O12 V5 V1 79.70(9) 2_556 . ? O10 V5 V1 78.05(9) . . ? O6 V5 V1 31.23(7) . . ? O13 V5 V1 42.88(7) . . ? O8 V5 V4 135.83(11) . 2_556 ? O5 V5 V4 33.07(8) . 2_556 ? O12 V5 V4 85.62(8) 2_556 2_556 ? O10 V5 V4 84.38(8) . 2_556 ? O6 V5 V4 123.23(8) . 2_556 ? O13 V5 V4 49.14(7) . 2_556 ? V1 V5 V4 92.01(3) . 2_556 ? O8 V5 V2 134.21(11) . 2_556 ? O5 V5 V2 82.53(9) . 2_556 ? O12 V5 V2 32.66(8) 2_556 2_556 ? O10 V5 V2 124.33(8) . 2_556 ? O6 V5 V2 81.68(8) . 2_556 ? O13 V5 V2 46.57(7) . 2_556 ? V1 V5 V2 62.50(3) . 2_556 ? V4 V5 V2 61.05(4) 2_556 2_556 ? O8 V5 V3 133.61(11) . . ? O5 V5 V3 81.02(9) . . ? O12 V5 V3 124.42(8) 2_556 . ? O10 V5 V3 32.52(8) . . ? O6 V5 V3 82.02(8) . . ? O13 V5 V3 45.88(7) . . ? V1 V5 V3 61.02(3) . . ? V4 V5 V3 60.24(3) 2_556 . ? V2 V5 V3 92.17(3) 2_556 . ? V2 O2 Na2 175.31(18) . . ? V1 O3 V4 111.94(13) . . ? V2 O4 V4 116.07(14) . . ? V5 O5 V4 114.29(14) . 2_556 ? V1 O6 V5 109.19(13) . . ? V1 O7 V2 106.84(12) . 2_556 ? V1 O7 V3 107.68(12) . 2_556 ? V2 O7 V3 100.81(11) 2_556 2_556 ? V1 O9 V3 106.62(12) . . ? V1 O9 V2 107.72(12) . . ? V3 O9 V2 100.47(11) . . ? V3 O10 V5 113.70(14) . . ? V3 O11 V4 114.24(14) . 2_556 ? V2 O12 V5 113.79(13) . 2_556 ? V1 O13 V1 101.78(11) . 2_556 ? V1 O13 V3 92.90(10) . . ? V1 O13 V3 94.65(10) 2_556 . ? V1 O13 V2 94.72(10) . 2_556 ? V1 O13 V2 91.77(10) 2_556 2_556 ? V3 O13 V2 168.83(13) . 2_556 ? V1 O13 V5 88.18(10) . . ? V1 O13 V5 169.88(13) 2_556 . ? V3 O13 V5 86.56(9) . . ? V2 O13 V5 85.54(9) 2_556 . ? V1 O13 V4 171.16(13) . 2_556 ? V1 O13 V4 87.00(9) 2_556 2_556 ? V3 O13 V4 85.31(9) . 2_556 ? V2 O13 V4 85.92(9) 2_556 2_556 ? V5 O13 V4 83.08(9) . 2_556 ? O21 Al1 O21 179.998(1) . 2_666 ? O21 Al1 O19 89.12(15) . . ? O21 Al1 O19 90.88(15) 2_666 . ? O21 Al1 O19 90.88(15) . 2_666 ? O21 Al1 O19 89.12(15) 2_666 2_666 ? O19 Al1 O19 180.0 . 2_666 ? O21 Al1 O20 89.72(15) . . ? O21 Al1 O20 90.28(15) 2_666 . ? O19 Al1 O20 92.25(15) . . ? O19 Al1 O20 87.75(15) 2_666 . ? O21 Al1 O20 90.28(15) . 2_666 ? O21 Al1 O20 89.72(15) 2_666 2_666 ? O19 Al1 O20 87.75(15) . 2_666 ? O19 Al1 O20 92.25(15) 2_666 2_666 ? O20 Al1 O20 180.0(2) . 2_666 ? O23 Na1 O23 179.999(1) 2_657 . ? O23 Na1 O17 91.91(16) 2_657 2_657 ? O23 Na1 O17 88.09(16) . 2_657 ? O23 Na1 O17 88.09(16) 2_657 . ? O23 Na1 O17 91.91(16) . . ? O17 Na1 O17 180.000(1) 2_657 . ? O23 Na1 O15 95.84(19) 2_657 2_657 ? O23 Na1 O15 84.16(19) . 2_657 ? O17 Na1 O15 81.78(14) 2_657 2_657 ? O17 Na1 O15 98.22(14) . 2_657 ? O23 Na1 O15 84.16(19) 2_657 . ? O23 Na1 O15 95.84(19) . . ? O17 Na1 O15 98.22(14) 2_657 . ? O17 Na1 O15 81.78(14) . . ? O15 Na1 O15 180.0 2_657 . ? O23 Na1 Na2 87.24(13) 2_657 . ? O23 Na1 Na2 92.76(13) . . ? O17 Na1 Na2 138.21(10) 2_657 . ? O17 Na1 Na2 41.79(10) . . ? O15 Na1 Na2 139.90(11) 2_657 . ? O15 Na1 Na2 40.10(11) . . ? O23 Na1 Na2 92.76(13) 2_657 2_657 ? O23 Na1 Na2 87.24(13) . 2_657 ? O17 Na1 Na2 41.79(10) 2_657 2_657 ? O17 Na1 Na2 138.21(10) . 2_657 ? O15 Na1 Na2 40.10(11) 2_657 2_657 ? O15 Na1 Na2 139.90(11) . 2_657 ? Na2 Na1 Na2 180.0 . 2_657 ? O16 Na2 O15 174.36(19) . . ? O16 Na2 O18 87.53(16) . . ? O15 Na2 O18 88.68(19) . . ? O16 Na2 O2 94.57(13) . . ? O15 Na2 O2 89.59(16) . . ? O18 Na2 O2 174.39(15) . . ? O16 Na2 O17 92.27(15) . . ? O15 Na2 O17 83.87(15) . . ? O18 Na2 O17 94.63(16) . . ? O2 Na2 O17 90.49(14) . . ? O16 Na2 O22 87.42(15) . . ? O15 Na2 O22 97.32(16) . . ? O18 Na2 O22 99.29(16) . . ? O2 Na2 O22 75.64(13) . . ? O17 Na2 O22 166.05(16) . . ? O16 Na2 Na1 134.00(13) . . ? O15 Na2 Na1 42.26(12) . . ? O18 Na2 Na1 94.74(12) . . ? O2 Na2 Na1 87.55(9) . . ? O17 Na2 Na1 41.73(9) . . ? O22 Na2 Na1 136.86(11) . . ? Na2 O15 Na1 97.64(17) . . ? Na1 O17 Na2 96.47(14) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.44 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.767 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.130