 
data_1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          
'[Zn (H2 O)2]2[Na (H2 O)3][V12 B16 O50 (O H)8], 7(H3 O), 4(H2 O)' 
_chemical_formula_sum 
 'B16 H51 Na O76 V12 Zn2 ' 
_chemical_formula_weight          2205.37 
 
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' 
 'B'  'B'   0.0013   0.0007 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 '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' 
 'V'  'V'   0.3005   0.5294 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Zn'  'Zn'   0.2839   1.4301 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    C2/c
_symmetry_space_group_name_Hall   'C 2yc '  
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    17.048(8) 
_cell_length_b                    17.431(8) 
_cell_length_c                    23.628(11) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.063(8) 
_cell_angle_gamma                 90.00 
_cell_volume                      7021(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        BLOCK 
_exptl_crystal_colour             black 
_exptl_crystal_size_max           0.11 
_exptl_crystal_size_mid           0.09 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.038 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              4140 
_exptl_absorpt_coefficient_mu     2.325 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.5879 
_exptl_absorpt_correction_T_max   0.6718 
_exptl_absorpt_process_details     
 'Jacobson, R. (1998) Private communication'
 
_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   'Rigaku Mercury'
_diffrn_measurement_method        ω
_diffrn_detector_area_resol_mean  7.31 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             22041 
_diffrn_reflns_av_R_equivalents   0.0270 
_diffrn_reflns_av_sigmaI/netI     0.0299 
_diffrn_reflns_limit_h_min        -21 
_diffrn_reflns_limit_h_max        21 
_diffrn_reflns_limit_k_min        -21 
_diffrn_reflns_limit_k_max        21 
_diffrn_reflns_limit_l_min        -29 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          1.67 
_diffrn_reflns_theta_max          26.50 
_reflns_number_total              7202 
_reflns_number_gt                 6026 
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1293P)²+119.6116P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    '_' 
_refine_ls_hydrogen_treatment     none 
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          7202 
_refine_ls_number_parameters      570 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0826 
_refine_ls_R_factor_gt            0.0721 
_refine_ls_wR_factor_ref          0.2196 
_refine_ls_wR_factor_gt           0.2080 
_refine_ls_goodness_of_fit_ref    1.036 
_refine_ls_restrained_S_all       1.036 
_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 
B1 B 0.3771(4) 0.2889(4) 0.4108(3) 0.0189(13) Uani 1 1 d . . 1 
B2 B 0.6471(4) 0.1418(4) 0.3177(3) 0.0216(14) Uani 1 1 d . . 1 
B3 B 0.6415(5) 0.2965(5) 0.4910(4) 0.0320(18) Uani 1 1 d . . 1 
B4 B 0.6380(4) 0.2391(5) 0.3946(3) 0.0239(15) Uani 1 1 d . . 1 
B5 B 0.5185(4) 0.3079(4) 0.4340(3) 0.0220(14) Uani 1 1 d . . 1 
B6 B 0.3279(4) 0.4570(4) 0.2647(3) 0.0222(14) Uani 1 1 d . . 1 
B7 B 0.2318(4) 0.3039(5) 0.4246(3) 0.0252(15) Uani 1 1 d . . 1 
B8 B 0.2929(4) 0.3574(4) 0.3380(3) 0.0211(14) Uani 1 1 d . . 1 
V1 V 0.28470(6) 0.29895(6) 0.21518(5) 0.0212(3) Uani 1 1 d . . 1 
V2 V 0.55251(6) 0.44201(6) 0.13766(5) 0.0209(3) Uani 1 1 d . . 1 
V3 V 0.37887(6) 0.40893(6) 0.14372(4) 0.0219(3) Uani 1 1 d . . 1 
V4 V 0.32834(6) 0.18866(6) 0.30929(4) 0.0188(2) Uani 1 1 d . . 1 
V5 V 0.5000 0.50428(8) 0.2500 0.0222(3) Uani 1 2 d S . 1 
V6 V 0.48205(6) 0.15634(6) 0.36868(4) 0.0195(3) Uani 1 1 d . . 1 
V7 V 0.5000 0.09415(8) 0.2500 0.0197(3) Uani 1 2 d S . 1 
Zn1 Zn 0.6857(5) -0.0284(4) 0.35621(18) 0.0356(11) Uani 0.75(4) 1 d P . 1 
O1 O 0.3248(3) 0.4568(3) 0.0993(2) 0.0413(13) Uani 1 1 d . A 1 
O2 O 0.5000 0.5973(4) 0.2500 0.044(2) Uani 1 2 d S B 1 
O3 O 0.5789(3) 0.5118(3) 0.0960(2) 0.0391(13) Uani 1 1 d . C 1 
O4 O 0.6673(3) 0.1663(3) 0.37413(19) 0.0266(10) Uani 1 1 d . . 1 
O5 O 0.5000 0.0008(4) 0.2500 0.0338(16) Uani 1 2 d S D 1 
O6 O 0.2239(3) 0.3452(3) 0.3764(2) 0.0282(10) Uani 1 1 d . . 1 
O7 O 0.4791(3) 0.0871(3) 0.4149(2) 0.0368(12) Uani 1 1 d . . 1 
O8 O 0.4083(3) 0.4611(3) 0.28673(19) 0.0257(10) Uani 1 1 d . . 1 
O9 O 0.6778(3) 0.0631(3) 0.3073(2) 0.0363(12) Uani 1 1 d . . 1 
O10 O 0.5609(3) 0.1381(3) 0.31164(19) 0.0232(9) Uani 1 1 d . . 1 
O11 O 0.5500(2) 0.2382(3) 0.40361(18) 0.0214(9) Uani 1 1 d . . 1 
O12 O 0.3223(3) 0.4046(3) 0.21616(19) 0.0269(10) Uani 1 1 d . . 1 
O13 O 0.3662(2) 0.3598(2) 0.37343(18) 0.0200(9) Uani 1 1 d . . 1 
O14 O 0.6565(3) 0.3028(3) 0.35483(19) 0.0245(10) Uani 1 1 d . . 1 
O15 O 0.4179(3) 0.1213(3) 0.30419(19) 0.0227(9) Uani 1 1 d . . 1 
O16 O 0.3917(2) 0.2232(3) 0.37396(18) 0.0206(9) Uani 1 1 d . . 1 
O18 O 0.2977(3) 0.2947(3) 0.29713(19) 0.0230(9) Uani 1 1 d . . 1 
O19 O 0.4384(2) 0.2989(3) 0.45169(18) 0.0212(9) Uani 1 1 d . . 1 
O20 O 0.2762(3) 0.4303(3) 0.31125(19) 0.0230(9) Uani 1 1 d . . 1 
O21 O 0.5425(3) 0.4764(3) 0.32431(19) 0.0250(9) Uani 1 1 d . . 1 
O22 O 0.6808(3) 0.1933(3) 0.27343(18) 0.0231(9) Uani 1 1 d . . 1 
O23 O 0.6772(3) 0.2551(3) 0.4498(2) 0.0328(12) Uani 1 1 d . . 1 
O24 O 0.5659(3) 0.3220(3) 0.4860(2) 0.0300(11) Uani 1 1 d . . 1 
O25 O 0.1915(3) 0.2999(3) 0.2009(2) 0.0370(12) Uani 1 1 d . E 1 
O26 O 0.2545(3) 0.1407(3) 0.3348(2) 0.0335(11) Uani 1 1 d . F 1 
O27 O 0.3025(3) 0.2765(3) 0.44254(19) 0.0244(9) Uani 1 1 d . . 1 
O28 O 0.3021(3) 0.5348(3) 0.2486(3) 0.0430(14) Uani 1 1 d . . 1 
O29 O 0.6806(4) 0.3151(5) 0.5397(3) 0.0567(19) Uani 1 1 d . . 1 
O30 O 0.1651(3) 0.2909(4) 0.4566(2) 0.0451(16) Uani 1 1 d . . 1 
Na1 Na 0.0321(4) 0.2390(6) 0.4479(3) 0.061(2) Uani 0.50 1 d P . 1 
O1W O 0.5000 0.3005(10) 0.2500 0.130(7) Uani 1 2 d S G 1 
O3W O 0.7302(14) 0.0201(11) 0.4267(6) 0.053(5) Uani 0.75(4) 1 d P . 1 
O4W O 0.6068(11) -0.1010(11) 0.2840(12) 0.111(8) Uani 0.50 1 d P H 1 
O7W O 0.0893(8) 0.1372(7) 0.3692(6) 0.056(3) Uani 0.50 1 d P I 1 
O6W O -0.0200(12) 0.3635(12) 0.4704(7) 0.088(6) Uani 0.50 1 d P J 1 
O5W O -0.0347(16) 0.2724(17) 0.3619(12) 0.131(9) Uani 0.50 1 d P K 1 
O8W O 0.3419(7) -0.0262(6) 0.3210(6) 0.049(3) Uani 0.50 1 d P L 1 
O10A O 0.8491(8) 0.1454(6) 0.3419(5) 0.051(3) Uani 0.50 1 d P M 1 
O9W O -0.1720(6) 0.3699(8) 0.4222(5) 0.047(2) Uani 0.50 1 d P N 1 
O14W O -0.2126(10) 0.5819(8) 0.4464(5) 0.059(4) Uani 0.50 1 d P O 1 
O13W O 0.6031(11) -0.2368(19) 0.3028(9) 0.126(10) Uani 0.50 1 d P P 1 
O15W O 0.5740(8) 0.5402(8) -0.0040(6) 0.050(3) Uani 0.50 1 d P Q 1 
O11W O 0.3796(8) 0.4174(8) 0.5179(6) 0.050(3) Uani 0.50 1 d P R 1 
O2W O 0.5728(6) -0.0532(6) 0.3687(7) 0.050(4) Uani 0.75(4) 1 d P . 1 
Zn1' Zn 0.6690(13) -0.0444(14) 0.3433(17) 0.052(4) Uani 0.25(4) 1 d P . 2 
O2W' O 0.5795(17) -0.0409(17) 0.404(2) 0.050(11) Uani 0.25(4) 1 d P . 2 
O3W' O 0.698(3) 0.029(4) 0.429(3) 0.050(11) Uani 0.25(4) 1 d P . 2 
O9W' O -0.2045(6) 0.4739(8) 0.4167(5) 0.047(2) Uani 0.50 1 d P S 2 
O10B O 0.7818(10) 0.1188(9) 0.3929(6) 0.069(5) Uani 0.50 1 d P T 2 
O17 O 0.5264(3) 0.3759(3) 0.39621(19) 0.0247(9) Uani 1 1 d . . 1 
 
 
_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 
B1 O19 1.434(8) . ? 
B1 O16 1.460(8) . ? 
B1 O27 1.493(8) . ? 
B1 O13 1.530(8) . ? 
B2 O4 1.441(9) . ? 
B2 O10 1.478(8) . ? 
B2 O9 1.488(8) . ? 
B2 O22 1.495(9) . ? 
B3 O23 1.358(10) . ? 
B3 O29 1.367(10) . ? 
B3 O24 1.368(9) . ? 
B4 O4 1.446(9) . ? 
B4 O14 1.488(9) . ? 
B4 O23 1.491(8) . ? 
B4 O11 1.516(8) . ? 
B5 O19 1.437(8) . ? 
B5 O17 1.489(8) . ? 
B5 O24 1.491(8) . ? 
B5 O11 1.510(8) . ? 
B5 Na1 3.035(10) 7_556 ? 
B6 O8 1.468(9) . ? 
B6 O12 1.470(9) . ? 
B6 O28 1.476(8) . ? 
B6 O20 1.485(8) . ? 
B7 O6 1.353(9) . ? 
B7 O27 1.364(9) . ? 
B7 O30 1.383(9) . ? 
B8 O20 1.446(8) . ? 
B8 O18 1.461(9) . ? 
B8 O6 1.502(8) . ? 
B8 O13 1.504(8) . ? 
V1 O25 1.624(5) . ? 
V1 O14 1.936(5) 2_655 ? 
V1 O12 1.950(5) . ? 
V1 O18 1.950(5) . ? 
V1 O22 1.951(5) 2_655 ? 
V1 V3 3.0181(17) . ? 
V1 V4 3.0315(17) . ? 
V2 O3 1.629(5) . ? 
V2 O8 1.935(5) 2_655 ? 
V2 O17 1.943(5) 2_655 ? 
V2 O21 1.948(5) 2_655 ? 
V2 O13 2.011(5) 2_655 ? 
V2 V5 3.0050(16) . ? 
V2 V3 3.019(2) . ? 
V3 O1 1.626(5) . ? 
V3 O21 1.936(5) 2_655 ? 
V3 O14 1.946(5) 2_655 ? 
V3 O17 1.958(5) 2_655 ? 
V3 O12 1.967(5) . ? 
V4 O26 1.627(5) . ? 
V4 O15 1.929(5) . ? 
V4 O18 1.942(5) . ? 
V4 O22 1.962(5) 2_655 ? 
V4 O16 1.965(4) . ? 
V4 V6 3.0241(18) . ? 
V5 O2 1.622(7) . ? 
V5 O8 1.941(5) 2_655 ? 
V5 O8 1.941(5) . ? 
V5 O21 1.960(5) 2_655 ? 
V5 O21 1.960(5) . ? 
V5 V2 3.0050(16) 2_655 ? 
V6 O7 1.628(5) . ? 
V6 O10 1.931(4) . ? 
V6 O16 1.935(4) . ? 
V6 O15 1.972(5) . ? 
V6 O11 2.014(5) . ? 
V6 V7 3.0222(17) . ? 
V7 O5 1.628(7) . ? 
V7 O10 1.945(4) 2_655 ? 
V7 O10 1.945(4) . ? 
V7 O15 1.957(4) 2_655 ? 
V7 O15 1.957(4) . ? 
V7 V6 3.0222(17) 2_655 ? 
Zn1 O9 1.974(7) . ? 
Zn1 O2W 1.996(13) . ? 
Zn1 O20 2.007(6) 3_545 ? 
Zn1 O3W 2.015(16) . ? 
Zn1 O6 2.347(7) 3_545 ? 
O6 Zn1 2.347(7) 3_455 ? 
O8 V2 1.935(5) 2_655 ? 
O13 V2 2.011(4) 2_655 ? 
O14 V1 1.936(5) 2_655 ? 
O14 V3 1.946(5) 2_655 ? 
O19 Na1 2.513(9) 7_556 ? 
O20 Zn1 2.007(6) 3_455 ? 
O21 V3 1.936(5) 2_655 ? 
O21 V2 1.948(5) 2_655 ? 
O22 V1 1.951(5) 2_655 ? 
O22 V4 1.962(5) 2_655 ? 
O24 Na1 2.523(9) 7_556 ? 
O30 Na1 2.451(9) . ? 
Na1 O5W 2.40(3) . ? 
Na1 O6W 2.40(2) . ? 
Na1 O19 2.513(9) 7_556 ? 
Na1 O24 2.523(9) 7_556 ? 
Na1 O7W 2.751(17) . ? 
Na1 B5 3.035(10) 7_556 ? 
Zn1' O2W' 2.09(5) . ? 
Zn1' O3W' 2.43(8) . ? 
O17 V2 1.943(5) 2_655 ? 
O17 V3 1.958(5) 2_655 ? 
 
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 
O19 B1 O16 111.9(5) . . ? 
O19 B1 O27 107.4(5) . . ? 
O16 B1 O27 109.4(5) . . ? 
O19 B1 O13 112.2(5) . . ? 
O16 B1 O13 108.1(5) . . ? 
O27 B1 O13 107.7(5) . . ? 
O4 B2 O10 109.8(5) . . ? 
O4 B2 O9 110.0(5) . . ? 
O10 B2 O9 107.1(5) . . ? 
O4 B2 O22 112.2(6) . . ? 
O10 B2 O22 109.9(5) . . ? 
O9 B2 O22 107.7(5) . . ? 
O23 B3 O29 120.7(7) . . ? 
O23 B3 O24 122.2(6) . . ? 
O29 B3 O24 117.0(7) . . ? 
O4 B4 O14 111.8(5) . . ? 
O4 B4 O23 107.6(5) . . ? 
O14 B4 O23 108.4(6) . . ? 
O4 B4 O11 112.3(6) . . ? 
O14 B4 O11 107.9(5) . . ? 
O23 B4 O11 108.7(5) . . ? 
O19 B5 O17 110.4(5) . . ? 
O19 B5 O24 107.0(5) . . ? 
O17 B5 O24 108.3(6) . . ? 
O19 B5 O11 112.9(6) . . ? 
O17 B5 O11 108.9(5) . . ? 
O24 B5 O11 109.4(5) . . ? 
O19 B5 Na1 55.4(3) . 7_556 ? 
O17 B5 Na1 142.3(5) . 7_556 ? 
O24 B5 Na1 56.0(3) . 7_556 ? 
O11 B5 Na1 108.7(4) . 7_556 ? 
O8 B6 O12 111.4(5) . . ? 
O8 B6 O28 109.0(6) . . ? 
O12 B6 O28 110.5(6) . . ? 
O8 B6 O20 107.9(5) . . ? 
O12 B6 O20 110.2(5) . . ? 
O28 B6 O20 107.6(5) . . ? 
O6 B7 O27 122.3(6) . . ? 
O6 B7 O30 117.7(6) . . ? 
O27 B7 O30 120.0(6) . . ? 
O20 B8 O18 112.3(5) . . ? 
O20 B8 O6 103.6(5) . . ? 
O18 B8 O6 109.8(5) . . ? 
O20 B8 O13 112.5(5) . . ? 
O18 B8 O13 109.9(5) . . ? 
O6 B8 O13 108.5(5) . . ? 
O25 V1 O14 109.2(2) . 2_655 ? 
O25 V1 O12 108.4(3) . . ? 
O14 V1 O12 78.85(19) 2_655 . ? 
O25 V1 O18 108.5(2) . . ? 
O14 V1 O18 142.3(2) 2_655 . ? 
O12 V1 O18 89.26(19) . . ? 
O25 V1 O22 109.4(2) . 2_655 ? 
O14 V1 O22 89.68(19) 2_655 2_655 ? 
O12 V1 O22 142.2(2) . 2_655 ? 
O18 V1 O22 78.06(19) . 2_655 ? 
O25 V1 V3 113.5(2) . . ? 
O14 V1 V3 39.09(14) 2_655 . ? 
O12 V1 V3 39.79(14) . . ? 
O18 V1 V3 121.30(15) . . ? 
O22 V1 V3 121.08(14) 2_655 . ? 
O25 V1 V4 113.4(2) . . ? 
O14 V1 V4 121.44(14) 2_655 . ? 
O12 V1 V4 120.63(15) . . ? 
O18 V1 V4 38.73(13) . . ? 
O22 V1 V4 39.36(13) 2_655 . ? 
V3 V1 V4 133.07(5) . . ? 
O3 V2 O8 109.5(3) . 2_655 ? 
O3 V2 O17 112.7(3) . 2_655 ? 
O8 V2 O17 136.0(2) 2_655 2_655 ? 
O3 V2 O21 106.3(3) . 2_655 ? 
O8 V2 O21 78.9(2) 2_655 2_655 ? 
O17 V2 O21 78.3(2) 2_655 2_655 ? 
O3 V2 O13 105.2(2) . 2_655 ? 
O8 V2 O13 90.31(19) 2_655 2_655 ? 
O17 V2 O13 90.02(19) 2_655 2_655 ? 
O21 V2 O13 148.54(19) 2_655 2_655 ? 
O3 V2 V5 110.3(2) . . ? 
O8 V2 V5 39.23(14) 2_655 . ? 
O17 V2 V5 111.79(14) 2_655 . ? 
O21 V2 V5 39.89(14) 2_655 . ? 
O13 V2 V5 125.35(13) 2_655 . ? 
O3 V2 V3 116.3(2) . . ? 
O8 V2 V3 109.04(14) 2_655 . ? 
O17 V2 V3 39.46(14) 2_655 . ? 
O21 V2 V3 38.83(14) 2_655 . ? 
O13 V2 V3 123.08(13) 2_655 . ? 
V5 V2 V3 74.58(4) . . ? 
O1 V3 O21 109.4(3) . 2_655 ? 
O1 V3 O14 108.9(3) . 2_655 ? 
O21 V3 O14 141.7(2) 2_655 2_655 ? 
O1 V3 O17 107.9(3) . 2_655 ? 
O21 V3 O17 78.22(19) 2_655 2_655 ? 
O14 V3 O17 89.1(2) 2_655 2_655 ? 
O1 V3 O12 107.6(3) . . ? 
O21 V3 O12 91.3(2) 2_655 . ? 
O14 V3 O12 78.2(2) 2_655 . ? 
O17 V3 O12 144.4(2) 2_655 . ? 
O1 V3 V1 112.7(2) . . ? 
O21 V3 V1 122.41(14) 2_655 . ? 
O14 V3 V1 38.87(14) 2_655 . ? 
O17 V3 V1 121.48(15) 2_655 . ? 
O12 V3 V1 39.39(15) . . ? 
O1 V3 V2 115.3(2) . . ? 
O21 V3 V2 39.12(14) 2_655 . ? 
O14 V3 V2 119.08(14) 2_655 . ? 
O17 V3 V2 39.12(14) 2_655 . ? 
O12 V3 V2 122.01(15) . . ? 
V1 V3 V2 132.06(5) . . ? 
O26 V4 O15 108.8(2) . . ? 
O26 V4 O18 109.6(2) . . ? 
O15 V4 O18 141.47(19) . . ? 
O26 V4 O22 109.2(2) . 2_655 ? 
O15 V4 O22 91.45(19) . 2_655 ? 
O18 V4 O22 77.99(19) . 2_655 ? 
O26 V4 O16 107.1(2) . . ? 
O15 V4 O16 78.48(19) . . ? 
O18 V4 O16 88.35(19) . . ? 
O22 V4 O16 143.61(19) 2_655 . ? 
O26 V4 V6 113.8(2) . . ? 
O15 V4 V6 39.69(14) . . ? 
O18 V4 V6 118.59(14) . . ? 
O22 V4 V6 122.55(14) 2_655 . ? 
O16 V4 V6 38.80(13) . . ? 
O26 V4 V1 114.1(2) . . ? 
O15 V4 V1 122.24(14) . . ? 
O18 V4 V1 38.94(14) . . ? 
O22 V4 V1 39.09(14) 2_655 . ? 
O16 V4 V1 120.70(14) . . ? 
V6 V4 V1 132.09(4) . . ? 
O2 V5 O8 112.85(15) . 2_655 ? 
O2 V5 O8 112.85(15) . . ? 
O8 V5 O8 134.3(3) 2_655 . ? 
O2 V5 O21 104.35(14) . 2_655 ? 
O8 V5 O21 78.5(2) 2_655 2_655 ? 
O8 V5 O21 90.4(2) . 2_655 ? 
O2 V5 O21 104.35(14) . . ? 
O8 V5 O21 90.4(2) 2_655 . ? 
O8 V5 O21 78.5(2) . . ? 
O21 V5 O21 151.3(3) 2_655 . ? 
O2 V5 V2 111.17(3) . . ? 
O8 V5 V2 39.10(14) 2_655 . ? 
O8 V5 V2 119.71(15) . . ? 
O21 V5 V2 39.60(14) 2_655 . ? 
O21 V5 V2 126.26(14) . . ? 
O2 V5 V2 111.17(3) . 2_655 ? 
O8 V5 V2 119.71(15) 2_655 2_655 ? 
O8 V5 V2 39.10(14) . 2_655 ? 
O21 V5 V2 126.26(14) 2_655 2_655 ? 
O21 V5 V2 39.60(14) . 2_655 ? 
V2 V5 V2 137.65(7) . 2_655 ? 
O7 V6 O10 111.6(2) . . ? 
O7 V6 O16 112.2(2) . . ? 
O10 V6 O16 134.3(2) . . ? 
O7 V6 O15 105.7(3) . . ? 
O10 V6 O15 78.23(19) . . ? 
O16 V6 O15 78.17(18) . . ? 
O7 V6 O11 105.6(2) . . ? 
O10 V6 O11 90.11(19) . . ? 
O16 V6 O11 90.26(18) . . ? 
O15 V6 O11 148.69(19) . . ? 
O7 V6 V7 111.0(2) . . ? 
O10 V6 V7 38.93(13) . . ? 
O16 V6 V7 110.93(13) . . ? 
O15 V6 V7 39.53(13) . . ? 
O11 V6 V7 125.14(13) . . ? 
O7 V6 V4 115.0(2) . . ? 
O10 V6 V4 108.08(14) . . ? 
O16 V6 V4 39.51(13) . . ? 
O15 V6 V4 38.66(13) . . ? 
O11 V6 V4 123.77(13) . . ? 
V7 V6 V4 74.03(4) . . ? 
O5 V7 O10 113.21(14) . 2_655 ? 
O5 V7 O10 113.21(14) . . ? 
O10 V7 O10 133.6(3) 2_655 . ? 
O5 V7 O15 104.01(13) . 2_655 ? 
O10 V7 O15 78.26(19) 2_655 2_655 ? 
O10 V7 O15 90.73(19) . 2_655 ? 
O5 V7 O15 104.01(13) . . ? 
O10 V7 O15 90.73(19) 2_655 . ? 
O10 V7 O15 78.26(19) . . ? 
O15 V7 O15 152.0(3) 2_655 . ? 
O5 V7 V6 111.02(3) . . ? 
O10 V7 V6 119.92(15) 2_655 . ? 
O10 V7 V6 38.59(13) . . ? 
O15 V7 V6 126.41(14) 2_655 . ? 
O15 V7 V6 39.90(13) . . ? 
O5 V7 V6 111.02(3) . 2_655 ? 
O10 V7 V6 38.59(13) 2_655 2_655 ? 
O10 V7 V6 119.92(15) . 2_655 ? 
O15 V7 V6 39.90(13) 2_655 2_655 ? 
O15 V7 V6 126.41(14) . 2_655 ? 
V6 V7 V6 137.96(7) . 2_655 ? 
O9 Zn1 O2W 101.3(5) . . ? 
O9 Zn1 O20 91.9(3) . 3_545 ? 
O2W Zn1 O20 137.9(9) . 3_545 ? 
O9 Zn1 O3W 99.8(8) . . ? 
O2W Zn1 O3W 109.3(10) . . ? 
O20 Zn1 O3W 107.5(5) 3_545 . ? 
O9 Zn1 O6 153.7(3) . 3_545 ? 
O2W Zn1 O6 91.9(4) . 3_545 ? 
O20 Zn1 O6 63.7(2) 3_545 3_545 ? 
O3W Zn1 O6 97.0(6) . 3_545 ? 
B2 O4 B4 119.1(5) . . ? 
B7 O6 B8 120.5(5) . . ? 
B7 O6 Zn1 134.3(5) . 3_455 ? 
B8 O6 Zn1 87.7(4) . 3_455 ? 
B6 O8 V2 129.8(4) . 2_655 ? 
B6 O8 V5 127.8(4) . . ? 
V2 O8 V5 101.7(2) 2_655 . ? 
B2 O9 Zn1 132.2(4) . . ? 
B2 O10 V6 128.2(4) . . ? 
B2 O10 V7 128.3(4) . . ? 
V6 O10 V7 102.5(2) . . ? 
B5 O11 B4 114.3(5) . . ? 
B5 O11 V6 124.1(4) . . ? 
B4 O11 V6 121.2(4) . . ? 
B6 O12 V1 128.1(4) . . ? 
B6 O12 V3 128.6(4) . . ? 
V1 O12 V3 100.8(2) . . ? 
B8 O13 B1 113.5(5) . . ? 
B8 O13 V2 121.3(4) . 2_655 ? 
B1 O13 V2 124.6(4) . 2_655 ? 
B4 O14 V1 128.5(4) . 2_655 ? 
B4 O14 V3 129.3(4) . 2_655 ? 
V1 O14 V3 102.0(2) 2_655 2_655 ? 
V4 O15 V7 139.0(2) . . ? 
V4 O15 V6 101.6(2) . . ? 
V7 O15 V6 100.6(2) . . ? 
B1 O16 V6 130.3(4) . . ? 
B1 O16 V4 127.6(4) . . ? 
V6 O16 V4 101.7(2) . . ? 
B8 O18 V4 129.1(4) . . ? 
B8 O18 V1 128.4(4) . . ? 
V4 O18 V1 102.3(2) . . ? 
B1 O19 B5 120.6(5) . . ? 
B1 O19 Na1 138.5(4) . 7_556 ? 
B5 O19 Na1 96.6(4) . 7_556 ? 
B8 O20 B6 118.9(5) . . ? 
B8 O20 Zn1 103.6(4) . 3_455 ? 
B6 O20 Zn1 137.4(4) . 3_455 ? 
V3 O21 V2 102.0(2) 2_655 2_655 ? 
V3 O21 V5 139.1(2) 2_655 . ? 
V2 O21 V5 100.5(2) 2_655 . ? 
B2 O22 V1 125.9(4) . 2_655 ? 
B2 O22 V4 130.0(4) . 2_655 ? 
V1 O22 V4 101.6(2) 2_655 2_655 ? 
B3 O23 B4 121.8(5) . . ? 
B3 O24 B5 121.8(5) . . ? 
B3 O24 Na1 115.7(5) . 7_556 ? 
B5 O24 Na1 94.7(4) . 7_556 ? 
B7 O27 B1 123.1(5) . . ? 
B7 O30 Na1 140.9(6) . . ? 
O5W Na1 O6W 78.1(8) . . ? 
O5W Na1 O30 114.8(8) . . ? 
O6W Na1 O30 89.4(6) . . ? 
O5W Na1 O19 163.2(8) . 7_556 ? 
O6W Na1 O19 95.9(5) . 7_556 ? 
O30 Na1 O19 80.5(3) . 7_556 ? 
O5W Na1 O24 108.2(8) . 7_556 ? 
O6W Na1 O24 90.0(6) . 7_556 ? 
O30 Na1 O24 135.9(4) . 7_556 ? 
O19 Na1 O24 55.7(2) 7_556 7_556 ? 
O5W Na1 O7W 75.6(8) . . ? 
O6W Na1 O7W 149.7(6) . . ? 
O30 Na1 O7W 88.1(4) . . ? 
O19 Na1 O7W 113.5(5) 7_556 . ? 
O24 Na1 O7W 112.5(5) 7_556 . ? 
O5W Na1 B5 135.2(8) . 7_556 ? 
O6W Na1 B5 86.3(5) . 7_556 ? 
O30 Na1 B5 106.7(3) . 7_556 ? 
O19 Na1 B5 28.06(18) 7_556 7_556 ? 
O24 Na1 B5 29.32(19) 7_556 7_556 ? 
O7W Na1 B5 123.3(5) . 7_556 ? 
O2W' Zn1' O3W' 64(3) . . ? 
B5 O17 V2 131.0(4) . 2_655 ? 
B5 O17 V3 126.7(4) . 2_655 ? 
V2 O17 V3 101.4(2) 2_655 2_655 ? 
 
_diffrn_measured_fraction_theta_max    0.989 
_diffrn_reflns_theta_full              26.50 
_diffrn_measured_fraction_theta_full   0.989 
_refine_diff_density_max    2.300 
_refine_diff_density_min   -2.553 
_refine_diff_density_rms    0.210 
