data_nash 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'H10 Ca1.33 Na1.33 O36 V6.67' 
_chemical_formula_weight          1009.77 
 
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' 
 'Ca'  'Ca'   0.2262   0.3064 
 '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' 
 'V'  'V'   0.3005   0.5294 
 '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+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
 
_cell_length_a                    10.0099(3) 
_cell_length_b                    21.8472(7) 
_cell_length_c                    11.1504(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  116.584(8) 
_cell_angle_gamma                 90.00 
_cell_volume                      2180.67(17) 
_cell_formula_units_Z             3 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.11 
_exptl_crystal_size_mid           0.09 
_exptl_crystal_size_min           0.05 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.307 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1478 
_exptl_absorpt_coefficient_mu     2.437 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   0.7753 
_exptl_absorpt_correction_T_max   0.8878 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71075 
_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_reflns_number             17847 
_diffrn_reflns_av_R_equivalents   0.0407 
_diffrn_reflns_av_sigmaI/netI     0.0294 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        26 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          3.46 
_diffrn_reflns_theta_max          25.02 
_reflns_number_total              3849 
_reflns_number_gt                 3144 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_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^)+(0.0295P)^2^+2.2707P] 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          3849 
_refine_ls_number_parameters      380 
_refine_ls_number_restraints      36 
_refine_ls_R_factor_all           0.0404 
_refine_ls_R_factor_gt            0.0293 
_refine_ls_wR_factor_ref          0.0708 
_refine_ls_wR_factor_gt           0.0679 
_refine_ls_goodness_of_fit_ref    1.092 
_refine_ls_restrained_S_all       1.095 
_refine_ls_shift/su_max           0.043 
_refine_ls_shift/su_mean          0.001 
 
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 0.66529(6) 0.00082(2) 0.49774(5) 0.01536(13) Uani 1 1 d . . . 
V2 V 0.40854(6) -0.09272(2) 0.32069(5) 0.01642(14) Uani 1 1 d . . . 
V3 V 0.37017(6) 0.04485(2) 0.24803(5) 0.01721(14) Uani 1 1 d . . . 
V4 V 0.61514(6) 0.13848(2) 0.42490(5) 0.01853(14) Uani 1 1 d . . . 
V5 V 0.69161(6) -0.13726(3) 0.57045(5) 0.01877(14) Uani 1 1 d . . . 
Ca Ca 0.21384(7) -0.06266(3) -0.07176(7) 0.02013(16) Uani 1 1 d . . . 
Na Na 0.66412(16) 0.30409(7) 0.31612(15) 0.0358(4) Uani 1 1 d . . . 
O1 O 0.7841(2) -0.05891(10) 0.5290(2) 0.0205(5) Uani 1 1 d . . . 
O2 O 0.7483(2) 0.06185(10) 0.4645(2) 0.0202(5) Uani 1 1 d . . . 
O3 O 0.5317(2) -0.01927(9) 0.3179(2) 0.0166(5) Uani 1 1 d . . . 
O4 O 0.7148(2) 0.02066(9) 0.6792(2) 0.0154(5) Uani 1 1 d . . . 
O5 O 0.4819(2) 0.06038(9) 0.4678(2) 0.0159(5) Uani 1 1 d . . . 
O6 O 0.3300(2) -0.10682(10) 0.1609(2) 0.0211(5) Uani 1 1 d . . . 
O7 O 0.3104(2) -0.14156(10) 0.3853(2) 0.0189(5) Uani 1 1 d . . . 
O8 O 0.5771(2) -0.13960(10) 0.3836(2) 0.0198(5) Uani 1 1 d . . . 
O9 O 0.2922(3) 0.02272(10) 0.0927(2) 0.0225(5) Uani 1 1 d . . . 
O10 O 0.2403(2) 0.09909(10) 0.2584(2) 0.0197(5) Uani 1 1 d . . . 
O11 O 0.5057(3) 0.10108(10) 0.2534(2) 0.0204(5) Uani 1 1 d . . . 
O12 O 0.7158(3) 0.18815(11) 0.3957(2) 0.0263(6) Uani 1 1 d . . . 
O13 O 0.4456(2) 0.18244(10) 0.4022(2) 0.0197(5) Uani 1 1 d . . . 
O14 O 0.8244(3) -0.18521(11) 0.5953(2) 0.0271(6) Uani 1 1 d . . . 
OW1 O 0.0166(3) -0.10090(11) -0.0240(3) 0.0261(6) Uani 1 1 d D . . 
H1A H 0.031(4) -0.1345(13) 0.026(3) 0.050 Uiso 1 1 d D . . 
H1B H -0.064(3) -0.1069(18) -0.101(2) 0.050 Uiso 1 1 d D . . 
OW2 O 0.4622(3) -0.09665(12) -0.0255(2) 0.0258(6) Uani 1 1 d D . . 
H2A H 0.473(4) -0.1015(19) -0.099(2) 0.050 Uiso 1 1 d D . . 
H2B H 0.534(4) -0.0739(17) 0.032(3) 0.050 Uiso 1 1 d D . . 
OW3 O 0.0200(3) 0.01659(12) -0.1547(3) 0.0318(6) Uani 1 1 d D . . 
H3A H -0.071(3) 0.0131(18) -0.217(3) 0.050 Uiso 1 1 d D . . 
H3B H 0.024(4) 0.0444(16) -0.096(3) 0.050 Uiso 1 1 d D . . 
OW4 O 0.0914(3) -0.08133(14) -0.3154(3) 0.0430(7) Uani 1 1 d D . . 
H4A H 0.142(3) -0.0721(19) -0.361(4) 0.050 Uiso 1 1 d D . . 
H4B H -0.003(2) -0.0716(19) -0.360(4) 0.050 Uiso 1 1 d D . . 
OW5 O 0.3190(3) 0.01924(12) -0.1627(2) 0.0306(6) Uani 1 1 d D . . 
H5A H 0.368(4) 0.0132(18) -0.210(3) 0.050 Uiso 1 1 d D . . 
H5B H 0.247(3) 0.0456(16) -0.206(4) 0.050 Uiso 1 1 d D . . 
OW6 O 0.1987(3) -0.17879(14) -0.1247(4) 0.0544(9) Uani 1 1 d D . . 
H6A H 0.263(3) -0.185(2) -0.037(2) 0.050 Uiso 1 1 d D . . 
H6B H 0.118(3) -0.1993(18) -0.126(4) 0.050 Uiso 1 1 d D . . 
OW7 O 0.9037(3) 0.30461(13) 0.3271(3) 0.0358(7) Uani 1 1 d D . . 
H7A H 0.907(4) 0.3194(18) 0.255(2) 0.050 Uiso 1 1 d D . . 
H7B H 0.955(4) 0.3289(16) 0.395(3) 0.050 Uiso 1 1 d D . . 
OW8 O 0.4376(3) 0.30653(11) 0.3329(2) 0.0278(6) Uani 1 1 d D . . 
H8A H 0.362(3) 0.3206(16) 0.261(3) 0.050 Uiso 1 1 d D . . 
H8B H 0.424(4) 0.2686(10) 0.350(4) 0.050 Uiso 1 1 d D . . 
OW9 O 0.5535(3) 0.25584(13) 0.1003(3) 0.0409(7) Uani 1 1 d D . . 
H9A H 0.467(3) 0.2395(17) 0.086(4) 0.050 Uiso 1 1 d D . . 
H9B H 0.614(3) 0.2298(15) 0.095(4) 0.050 Uiso 1 1 d D . . 
OW10 O 0.7885(3) 0.30880(13) 0.5604(3) 0.0356(6) Uani 1 1 d D . . 
H10A H 0.839(4) 0.3363(15) 0.619(3) 0.050 Uiso 1 1 d D . . 
H10B H 0.723(4) 0.2911(17) 0.581(4) 0.050 Uiso 1 1 d D . . 
OW11 O 0.5893(4) 0.39388(16) 0.1650(4) 0.0631(10) Uani 1 1 d D . . 
H11A H 0.533(4) 0.4030(19) 0.202(4) 0.050 Uiso 1 1 d D . . 
H11B H 0.593(5) 0.4178(17) 0.107(4) 0.050 Uiso 1 1 d D . . 
OW12 O 0.9289(3) -0.23440(11) 0.8589(3) 0.0359(6) Uani 1 1 d D . . 
H12A H 0.888(4) -0.2294(17) 0.771(2) 0.050 Uiso 1 1 d D . . 
H12B H 0.937(5) -0.2732(10) 0.877(4) 0.050 Uiso 1 1 d D . . 
Na2 Na 1.0570(3) -0.19273(16) 0.6099(4) 0.0526(15) Uani 0.496(6) 1 d P . . 
 
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 0.0226(3) 0.0134(3) 0.0139(3) -0.0012(2) 0.0116(2) -0.0023(2) 
V2 0.0247(3) 0.0137(3) 0.0132(3) -0.0029(2) 0.0105(2) -0.0037(2) 
V3 0.0277(3) 0.0139(3) 0.0138(3) -0.0014(2) 0.0127(2) -0.0031(2) 
V4 0.0280(3) 0.0141(3) 0.0180(3) -0.0015(2) 0.0143(3) -0.0052(2) 
V5 0.0263(3) 0.0159(3) 0.0162(3) -0.0011(2) 0.0113(2) 0.0006(2) 
Ca 0.0191(3) 0.0207(4) 0.0243(4) -0.0016(3) 0.0130(3) -0.0005(3) 
Na 0.0306(8) 0.0464(9) 0.0328(8) -0.0046(7) 0.0164(7) -0.0048(7) 
O1 0.0250(12) 0.0203(12) 0.0178(12) -0.0014(10) 0.0110(10) 0.0004(10) 
O2 0.0275(12) 0.0194(12) 0.0187(12) -0.0006(10) 0.0148(10) -0.0038(10) 
O3 0.0252(12) 0.0142(11) 0.0140(11) -0.0013(9) 0.0120(10) -0.0021(9) 
O4 0.0206(11) 0.0145(11) 0.0119(11) -0.0015(9) 0.0079(9) -0.0013(9) 
O5 0.0234(12) 0.0131(11) 0.0137(11) -0.0013(9) 0.0104(10) -0.0021(9) 
O6 0.0303(13) 0.0197(12) 0.0149(11) -0.0031(10) 0.0115(10) -0.0016(10) 
O7 0.0274(12) 0.0147(11) 0.0160(11) -0.0021(9) 0.0110(10) -0.0059(10) 
O8 0.0309(13) 0.0158(12) 0.0164(11) -0.0010(9) 0.0139(10) 0.0006(10) 
O9 0.0353(13) 0.0186(12) 0.0156(12) -0.0012(10) 0.0131(11) -0.0023(10) 
O10 0.0281(12) 0.0154(12) 0.0139(11) 0.0001(9) 0.0078(10) 0.0013(10) 
O11 0.0316(13) 0.0166(12) 0.0186(12) -0.0013(10) 0.0163(10) -0.0050(10) 
O12 0.0354(14) 0.0213(13) 0.0284(13) -0.0001(11) 0.0199(12) -0.0078(11) 
O13 0.0315(13) 0.0124(11) 0.0170(12) 0.0005(9) 0.0125(10) -0.0020(10) 
O14 0.0336(14) 0.0223(13) 0.0255(13) 0.0010(11) 0.0131(11) 0.0073(11) 
OW1 0.0197(12) 0.0244(13) 0.0341(15) 0.0042(11) 0.0119(11) -0.0002(10) 
OW2 0.0239(13) 0.0371(15) 0.0212(13) -0.0028(11) 0.0143(11) -0.0008(11) 
OW3 0.0240(13) 0.0326(15) 0.0380(16) -0.0044(13) 0.0132(12) 0.0037(12) 
OW4 0.0293(15) 0.0583(19) 0.0510(19) -0.0148(15) 0.0264(14) -0.0076(14) 
OW5 0.0302(14) 0.0402(16) 0.0299(15) -0.0011(12) 0.0211(12) -0.0025(12) 
OW6 0.0423(18) 0.0410(19) 0.083(2) -0.0182(18) 0.0306(18) -0.0077(15) 
OW7 0.0398(16) 0.0462(18) 0.0261(14) 0.0008(13) 0.0190(13) -0.0123(13) 
OW8 0.0255(13) 0.0227(13) 0.0288(14) 0.0033(11) 0.0062(11) 0.0037(11) 
OW9 0.0356(16) 0.0442(18) 0.0387(16) -0.0104(14) 0.0128(14) -0.0038(13) 
OW10 0.0378(16) 0.0378(17) 0.0321(15) -0.0150(13) 0.0163(13) -0.0094(13) 
OW11 0.075(3) 0.047(2) 0.073(3) 0.0090(19) 0.038(2) 0.0031(18) 
OW12 0.0528(17) 0.0204(14) 0.0321(15) 0.0073(12) 0.0170(14) 0.0021(13) 
Na2 0.032(2) 0.043(2) 0.093(3) -0.031(2) 0.037(2) -0.0133(15) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
V1 O1 1.693(2) . ? 
V1 O2 1.697(2) . ? 
V1 O3 1.898(2) . ? 
V1 O4 1.905(2) . ? 
V1 O5 2.148(2) 3_656 ? 
V1 O5 2.151(2) . ? 
V1 V4 3.0971(8) . ? 
V1 V5 3.1041(8) . ? 
V2 O6 1.622(2) . ? 
V2 O7 1.805(2) . ? 
V2 O8 1.824(2) . ? 
V2 O4 2.001(2) 3_656 ? 
V2 O3 2.032(2) . ? 
V2 O5 2.225(2) 3_656 ? 
V2 V3 3.0916(8) . ? 
V2 V5 3.1095(8) . ? 
V2 V4 3.1153(8) 3_656 ? 
V3 O9 1.623(2) . ? 
V3 O10 1.800(2) . ? 
V3 O11 1.811(2) . ? 
V3 O4 2.012(2) 3_656 ? 
V3 O3 2.014(2) . ? 
V3 O5 2.217(2) . ? 
V3 V5 3.1106(8) 3_656 ? 
V4 O12 1.610(2) . ? 
V4 O13 1.866(2) . ? 
V4 O7 1.905(2) 3_656 ? 
V4 O11 1.911(2) . ? 
V4 O2 2.061(2) . ? 
V4 O5 2.343(2) . ? 
V4 V5 3.0943(8) 3_656 ? 
V4 V2 3.1153(8) 3_656 ? 
V4 Na2 3.669(3) 3_756 ? 
V5 O14 1.616(2) . ? 
V5 O13 1.824(2) 3_656 ? 
V5 O8 1.876(2) . ? 
V5 O10 1.907(2) 3_656 ? 
V5 O1 2.094(2) . ? 
V5 O5 2.315(2) 3_656 ? 
V5 V4 3.0943(8) 3_656 ? 
V5 V3 3.1106(8) 3_656 ? 
Ca OW1 2.413(2) . ? 
Ca OW2 2.418(2) . ? 
Ca OW3 2.452(2) . ? 
Ca OW4 2.463(3) . ? 
Ca O9 2.484(2) . ? 
Ca OW5 2.509(3) . ? 
Ca O6 2.513(2) . ? 
Ca OW6 2.594(3) . ? 
Ca Na2 4.261(3) 1_454 ? 
Na OW7 2.346(3) . ? 
Na OW8 2.357(3) . ? 
Na OW9 2.397(3) . ? 
Na OW10 2.438(3) . ? 
Na OW11 2.473(4) . ? 
Na O12 2.657(3) . ? 
Na Na2 3.511(4) 3_756 ? 
O4 V2 2.001(2) 3_656 ? 
O4 V3 2.012(2) 3_656 ? 
O5 V1 2.148(2) 3_656 ? 
O5 V2 2.225(2) 3_656 ? 
O5 V5 2.315(2) 3_656 ? 
O7 V4 1.905(2) 3_656 ? 
O10 V5 1.908(2) 3_656 ? 
O12 Na2 2.305(4) 3_756 ? 
O13 V5 1.824(2) 3_656 ? 
O14 Na2 2.266(4) . ? 
OW4 Na2 2.546(4) 1_454 ? 
OW6 Na2 2.666(5) 1_454 ? 
OW7 Na2 2.525(5) 3_756 ? 
OW9 Na2 2.379(5) 2_655 ? 
Na2 O12 2.305(4) 3_756 ? 
Na2 OW9 2.379(5) 2_645 ? 
Na2 OW7 2.525(5) 3_756 ? 
Na2 OW4 2.546(4) 1_656 ? 
Na2 OW6 2.666(5) 1_656 ? 
Na2 Na 3.511(4) 3_756 ? 
Na2 V4 3.669(3) 3_756 ? 
Na2 Ca 4.261(3) 1_656 ? 
 
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 V1 O2 106.43(11) . . ? 
O1 V1 O3 97.87(10) . . ? 
O2 V1 O3 97.65(10) . . ? 
O1 V1 O4 97.57(10) . . ? 
O2 V1 O4 97.63(10) . . ? 
O3 V1 O4 154.20(9) . . ? 
O1 V1 O5 87.62(10) . 3_656 ? 
O2 V1 O5 165.95(10) . 3_656 ? 
O3 V1 O5 80.22(8) . 3_656 ? 
O4 V1 O5 79.91(8) . 3_656 ? 
O1 V1 O5 165.97(10) . . ? 
O2 V1 O5 87.59(10) . . ? 
O3 V1 O5 80.04(8) . . ? 
O4 V1 O5 79.98(8) . . ? 
O5 V1 O5 78.36(9) 3_656 . ? 
O1 V1 V4 144.96(8) . . ? 
O2 V1 V4 38.53(8) . . ? 
O3 V1 V4 89.57(7) . . ? 
O4 V1 V4 89.55(7) . . ? 
O5 V1 V4 127.42(6) 3_656 . ? 
O5 V1 V4 49.06(6) . . ? 
O1 V1 V5 39.44(8) . . ? 
O2 V1 V5 145.87(8) . . ? 
O3 V1 V5 89.35(7) . . ? 
O4 V1 V5 89.57(7) . . ? 
O5 V1 V5 48.18(6) 3_656 . ? 
O5 V1 V5 126.54(6) . . ? 
V4 V1 V5 175.60(2) . . ? 
O6 V2 O7 104.06(11) . . ? 
O6 V2 O8 103.07(11) . . ? 
O7 V2 O8 95.13(10) . . ? 
O6 V2 O4 98.87(10) . 3_656 ? 
O7 V2 O4 91.05(9) . 3_656 ? 
O8 V2 O4 154.97(9) . 3_656 ? 
O6 V2 O3 97.60(10) . . ? 
O7 V2 O3 156.27(9) . . ? 
O8 V2 O3 89.21(9) . . ? 
O4 V2 O3 75.99(9) 3_656 . ? 
O6 V2 O5 172.30(10) . 3_656 ? 
O7 V2 O5 82.11(9) . 3_656 ? 
O8 V2 O5 80.69(9) . 3_656 ? 
O4 V2 O5 76.17(8) 3_656 3_656 ? 
O3 V2 O5 75.59(8) . 3_656 ? 
O6 V2 V3 87.40(8) . . ? 
O7 V2 V3 130.80(7) . . ? 
O8 V2 V3 129.17(7) . . ? 
O4 V2 V3 39.75(6) 3_656 . ? 
O3 V2 V3 39.96(6) . . ? 
O5 V2 V3 85.04(6) 3_656 . ? 
O6 V2 V5 136.35(8) . . ? 
O7 V2 V5 84.16(7) . . ? 
O8 V2 V5 33.34(7) . . ? 
O4 V2 V5 124.11(6) 3_656 . ? 
O3 V2 V5 86.84(6) . . ? 
O5 V2 V5 47.98(6) 3_656 . ? 
V3 V2 V5 119.70(2) . . ? 
O6 V2 V4 137.88(8) . 3_656 ? 
O7 V2 V4 33.89(7) . 3_656 ? 
O8 V2 V4 84.47(7) . 3_656 ? 
O4 V2 V4 87.32(6) 3_656 3_656 ? 
O3 V2 V4 124.15(6) . 3_656 ? 
O5 V2 V4 48.60(5) 3_656 3_656 ? 
V3 V2 V4 119.96(2) . 3_656 ? 
V5 V2 V4 59.615(18) . 3_656 ? 
O9 V3 O10 104.40(11) . . ? 
O9 V3 O11 103.43(11) . . ? 
O10 V3 O11 95.93(10) . . ? 
O9 V3 O4 97.51(10) . 3_656 ? 
O10 V3 O4 89.68(9) . 3_656 ? 
O11 V3 O4 156.18(9) . 3_656 ? 
O9 V3 O3 97.17(10) . . ? 
O10 V3 O3 155.61(9) . . ? 
O11 V3 O3 89.94(9) . . ? 
O4 V3 O3 76.16(9) 3_656 . ? 
O9 V3 O5 171.46(10) . . ? 
O10 V3 O5 81.38(9) . . ? 
O11 V3 O5 81.95(9) . . ? 
O4 V3 O5 76.01(8) 3_656 . ? 
O3 V3 O5 76.02(8) . . ? 
O9 V3 V2 86.22(8) . . ? 
O10 V3 V2 129.17(7) . . ? 
O11 V3 V2 130.34(8) . . ? 
O4 V3 V2 39.50(6) 3_656 . ? 
O3 V3 V2 40.40(6) . . ? 
O5 V3 V2 85.24(6) . . ? 
O9 V3 V5 138.37(9) . 3_656 ? 
O10 V3 V5 34.07(7) . 3_656 ? 
O11 V3 V5 84.41(7) . 3_656 ? 
O4 V3 V5 87.47(6) 3_656 3_656 ? 
O3 V3 V5 123.97(6) . 3_656 ? 
O5 V3 V5 47.98(6) . 3_656 ? 
V2 V3 V5 119.87(2) . 3_656 ? 
O12 V4 O13 103.83(11) . . ? 
O12 V4 O7 103.41(11) . 3_656 ? 
O13 V4 O7 90.71(10) . 3_656 ? 
O12 V4 O11 102.47(11) . . ? 
O13 V4 O11 90.30(10) . . ? 
O7 V4 O11 153.06(9) 3_656 . ? 
O12 V4 O2 100.82(11) . . ? 
O13 V4 O2 155.34(9) . . ? 
O7 V4 O2 84.06(9) 3_656 . ? 
O11 V4 O2 83.87(9) . . ? 
O12 V4 O5 175.55(11) . . ? 
O13 V4 O5 80.57(8) . . ? 
O7 V4 O5 76.97(8) 3_656 . ? 
O11 V4 O5 76.65(8) . . ? 
O2 V4 O5 74.77(8) . . ? 
O12 V4 V5 136.43(9) . 3_656 ? 
O13 V4 V5 32.60(7) . 3_656 ? 
O7 V4 V5 83.08(7) 3_656 3_656 ? 
O11 V4 V5 83.37(7) . 3_656 ? 
O2 V4 V5 122.74(6) . 3_656 ? 
O5 V4 V5 47.98(5) . 3_656 ? 
O12 V4 V1 131.68(9) . . ? 
O13 V4 V1 124.48(7) . . ? 
O7 V4 V1 78.81(7) 3_656 . ? 
O11 V4 V1 78.48(7) . . ? 
O2 V4 V1 30.86(6) . . ? 
O5 V4 V1 43.90(5) . . ? 
V5 V4 V1 91.88(2) 3_656 . ? 
O12 V4 V2 135.24(9) . 3_656 ? 
O13 V4 V2 81.56(7) . 3_656 ? 
O7 V4 V2 31.89(6) 3_656 3_656 ? 
O11 V4 V2 122.08(7) . 3_656 ? 
O2 V4 V2 81.35(6) . 3_656 ? 
O5 V4 V2 45.44(5) . 3_656 ? 
V5 V4 V2 60.099(19) 3_656 3_656 ? 
V1 V4 V2 61.249(17) . 3_656 ? 
O12 V4 Na2 24.60(10) . 3_756 ? 
O13 V4 Na2 128.44(9) . 3_756 ? 
O7 V4 Na2 100.49(9) 3_656 3_756 ? 
O11 V4 Na2 99.88(9) . 3_756 ? 
O2 V4 Na2 76.22(8) . 3_756 ? 
O5 V4 Na2 150.98(8) . 3_756 ? 
V5 V4 Na2 161.03(6) 3_656 3_756 ? 
V1 V4 Na2 107.08(6) . 3_756 ? 
V2 V4 Na2 129.49(7) 3_656 3_756 ? 
O14 V5 O13 104.10(12) . 3_656 ? 
O14 V5 O8 102.69(11) . . ? 
O13 V5 O8 92.23(10) 3_656 . ? 
O14 V5 O10 102.35(11) . 3_656 ? 
O13 V5 O10 91.61(10) 3_656 3_656 ? 
O8 V5 O10 152.90(10) . 3_656 ? 
O14 V5 O1 99.02(11) . . ? 
O13 V5 O1 156.86(10) 3_656 . ? 
O8 V5 O1 83.57(9) . . ? 
O10 V5 O1 82.43(9) 3_656 . ? 
O14 V5 O5 173.67(11) . 3_656 ? 
O13 V5 O5 82.20(9) 3_656 3_656 ? 
O8 V5 O5 77.30(8) . 3_656 ? 
O10 V5 O5 76.67(8) 3_656 3_656 ? 
O1 V5 O5 74.67(8) . 3_656 ? 
O14 V5 V4 137.55(9) . 3_656 ? 
O13 V5 V4 33.45(7) 3_656 3_656 ? 
O8 V5 V4 84.29(7) . 3_656 ? 
O10 V5 V4 84.25(7) 3_656 3_656 ? 
O1 V5 V4 123.43(6) . 3_656 ? 
O5 V5 V4 48.76(5) 3_656 3_656 ? 
O14 V5 V1 129.93(9) . . ? 
O13 V5 V1 125.96(7) 3_656 . ? 
O8 V5 V1 78.36(7) . . ? 
O10 V5 V1 77.70(7) 3_656 . ? 
O1 V5 V1 30.92(6) . . ? 
O5 V5 V1 43.76(5) 3_656 . ? 
V4 V5 V1 92.51(2) 3_656 . ? 
O14 V5 V2 134.94(9) . . ? 
O13 V5 V2 82.33(7) 3_656 . ? 
O8 V5 V2 32.31(7) . . ? 
O10 V5 V2 122.25(7) 3_656 . ? 
O1 V5 V2 82.07(6) . . ? 
O5 V5 V2 45.58(5) 3_656 . ? 
V4 V5 V2 60.285(18) 3_656 . ? 
V1 V5 V2 61.649(17) . . ? 
O14 V5 V3 134.19(9) . 3_656 ? 
O13 V5 V3 81.88(7) 3_656 3_656 ? 
O8 V5 V3 122.66(7) . 3_656 ? 
O10 V5 V3 31.92(7) 3_656 3_656 ? 
O1 V5 V3 81.34(6) . 3_656 ? 
O5 V5 V3 45.36(5) 3_656 3_656 ? 
V4 V5 V3 60.456(18) 3_656 3_656 ? 
V1 V5 V3 61.369(17) . 3_656 ? 
V2 V5 V3 90.73(2) . 3_656 ? 
OW1 Ca OW2 135.32(9) . . ? 
OW1 Ca OW3 74.94(9) . . ? 
OW2 Ca OW3 149.50(9) . . ? 
OW1 Ca OW4 97.67(9) . . ? 
OW2 Ca OW4 98.13(9) . . ? 
OW3 Ca OW4 77.39(10) . . ? 
OW1 Ca O9 96.70(8) . . ? 
OW2 Ca O9 96.77(8) . . ? 
OW3 Ca O9 71.54(8) . . ? 
OW4 Ca O9 140.83(9) . . ? 
OW1 Ca OW5 150.35(9) . . ? 
OW2 Ca OW5 74.23(9) . . ? 
OW3 Ca OW5 75.42(9) . . ? 
OW4 Ca OW5 76.35(9) . . ? 
O9 Ca OW5 73.24(8) . . ? 
OW1 Ca O6 71.66(8) . . ? 
OW2 Ca O6 72.86(8) . . ? 
OW3 Ca O6 125.66(9) . . ? 
OW4 Ca O6 147.89(9) . . ? 
O9 Ca O6 71.26(7) . . ? 
OW5 Ca O6 127.40(8) . . ? 
OW1 Ca OW6 75.00(9) . . ? 
OW2 Ca OW6 72.42(9) . . ? 
OW3 Ca OW6 130.48(9) . . ? 
OW4 Ca OW6 68.75(11) . . ? 
O9 Ca OW6 150.40(10) . . ? 
OW5 Ca OW6 126.73(10) . . ? 
O6 Ca OW6 79.18(10) . . ? 
OW1 Ca Na2 85.42(8) . 1_454 ? 
OW2 Ca Na2 86.18(7) . 1_454 ? 
OW3 Ca Na2 102.85(8) . 1_454 ? 
OW4 Ca Na2 32.31(9) . 1_454 ? 
O9 Ca Na2 173.13(8) . 1_454 ? 
OW5 Ca Na2 101.75(8) . 1_454 ? 
O6 Ca Na2 115.59(8) . 1_454 ? 
OW6 Ca Na2 36.47(10) . 1_454 ? 
OW7 Na OW8 173.08(11) . . ? 
OW7 Na OW9 93.25(11) . . ? 
OW8 Na OW9 93.50(10) . . ? 
OW7 Na OW10 86.71(10) . . ? 
OW8 Na OW10 86.50(10) . . ? 
OW9 Na OW10 156.33(12) . . ? 
OW7 Na OW11 91.29(12) . . ? 
OW8 Na OW11 91.56(12) . . ? 
OW9 Na OW11 78.58(12) . . ? 
OW10 Na OW11 125.10(13) . . ? 
OW7 Na O12 86.88(10) . . ? 
OW8 Na O12 92.60(9) . . ? 
OW9 Na O12 81.34(10) . . ? 
OW10 Na O12 75.02(9) . . ? 
OW11 Na O12 159.69(12) . . ? 
OW7 Na Na2 45.94(9) . 3_756 ? 
OW8 Na Na2 133.52(10) . 3_756 ? 
OW9 Na Na2 83.84(10) . 3_756 ? 
OW10 Na Na2 79.16(10) . 3_756 ? 
OW11 Na Na2 132.54(12) . 3_756 ? 
O12 Na Na2 41.03(8) . 3_756 ? 
V1 O1 V5 109.65(11) . . ? 
V1 O2 V4 110.61(12) . . ? 
V1 O3 V3 108.17(10) . . ? 
V1 O3 V2 108.16(10) . . ? 
V3 O3 V2 99.63(9) . . ? 
V1 O4 V2 108.20(10) . 3_656 ? 
V1 O4 V3 108.09(10) . 3_656 ? 
V2 O4 V3 100.75(10) 3_656 3_656 ? 
V1 O5 V1 101.64(9) 3_656 . ? 
V1 O5 V3 93.18(8) 3_656 . ? 
V1 O5 V3 93.02(8) . . ? 
V1 O5 V2 93.43(8) 3_656 3_656 ? 
V1 O5 V2 92.63(8) . 3_656 ? 
V3 O5 V2 170.27(11) . 3_656 ? 
V1 O5 V5 88.06(8) 3_656 3_656 ? 
V1 O5 V5 170.29(11) . 3_656 ? 
V3 O5 V5 86.66(7) . 3_656 ? 
V2 O5 V5 86.44(7) 3_656 3_656 ? 
V1 O5 V4 171.33(11) 3_656 . ? 
V1 O5 V4 87.03(8) . . ? 
V3 O5 V4 86.43(7) . . ? 
V2 O5 V4 85.96(7) 3_656 . ? 
V5 O5 V4 83.27(7) 3_656 . ? 
V2 O6 Ca 146.48(12) . . ? 
V2 O7 V4 114.22(11) . 3_656 ? 
V2 O8 V5 114.35(12) . . ? 
V3 O9 Ca 148.63(13) . . ? 
V3 O10 V5 114.02(11) . 3_656 ? 
V3 O11 V4 114.10(11) . . ? 
V4 O12 Na2 138.49(16) . 3_756 ? 
V4 O12 Na 131.63(13) . . ? 
Na2 O12 Na 89.80(12) 3_756 . ? 
V5 O13 V4 113.96(11) 3_656 . ? 
V5 O14 Na2 143.05(17) . . ? 
Ca OW4 Na2 116.55(16) . 1_454 ? 
Ca OW6 Na2 108.19(14) . 1_454 ? 
Na OW7 Na2 92.17(12) . 3_756 ? 
Na2 OW9 Na 125.71(16) 2_655 . ? 
O14 Na2 O12 171.6(2) . 3_756 ? 
O14 Na2 OW9 87.33(14) . 2_645 ? 
O12 Na2 OW9 91.36(16) 3_756 2_645 ? 
O14 Na2 OW7 96.72(15) . 3_756 ? 
O12 Na2 OW7 90.98(14) 3_756 3_756 ? 
OW9 Na2 OW7 76.28(13) 2_645 3_756 ? 
O14 Na2 OW4 86.45(14) . 1_656 ? 
O12 Na2 OW4 88.68(13) 3_756 1_656 ? 
OW9 Na2 OW4 135.2(2) 2_645 1_656 ? 
OW7 Na2 OW4 148.5(2) 3_756 1_656 ? 
O14 Na2 OW6 95.19(16) . 1_656 ? 
O12 Na2 OW6 89.07(14) 3_756 1_656 ? 
OW9 Na2 OW6 158.37(19) 2_645 1_656 ? 
OW7 Na2 OW6 82.09(15) 3_756 1_656 ? 
OW4 Na2 OW6 66.46(13) 1_656 1_656 ? 
O14 Na2 Na 138.61(16) . 3_756 ? 
O12 Na2 Na 49.17(9) 3_756 3_756 ? 
OW9 Na2 Na 82.80(11) 2_645 3_756 ? 
OW7 Na2 Na 41.90(8) 3_756 3_756 ? 
OW4 Na2 Na 127.50(13) 1_656 3_756 ? 
OW6 Na2 Na 81.15(12) 1_656 3_756 ? 
O14 Na2 V4 155.20(16) . 3_756 ? 
O12 Na2 V4 16.91(7) 3_756 3_756 ? 
OW9 Na2 V4 95.29(13) 2_645 3_756 ? 
OW7 Na2 V4 107.89(12) 3_756 3_756 ? 
OW4 Na2 V4 74.31(10) 1_656 3_756 ? 
OW6 Na2 V4 91.37(11) 1_656 3_756 ? 
Na Na2 V4 66.06(6) 3_756 3_756 ? 
O14 Na2 Ca 89.72(11) . 1_656 ? 
O12 Na2 Ca 89.62(11) 3_756 1_656 ? 
OW9 Na2 Ca 166.27(16) 2_645 1_656 ? 
OW7 Na2 Ca 117.41(14) 3_756 1_656 ? 
OW4 Na2 Ca 31.14(8) 1_656 1_656 ? 
OW6 Na2 Ca 35.34(8) 1_656 1_656 ? 
Na Na2 Ca 107.97(9) 3_756 1_656 ? 
V4 Na2 Ca 81.90(6) 3_756 1_656 ? 
 
_diffrn_measured_fraction_theta_max    0.998 
_diffrn_reflns_theta_full              25.02 
_diffrn_measured_fraction_theta_full   0.998 
_refine_diff_density_max    0.368 
_refine_diff_density_min   -0.434 
_refine_diff_density_rms    0.083