Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_nazn _database_code_CSD 155046 _audit_creation_date 'Wed Dec 13 2000' _audit_creation_method SHELXL ; ? ; _chemical_formula_sum 'Na4 O36 P8 V4 Zn4 H4' _chemical_formula_weight 1384.99 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' 'P' 'P' 0.1023 0.0942 '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 'P 21/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5441(2) _cell_length_b 8.9831(2) _cell_length_c 9.0836(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.2411(15) _cell_angle_gamma 90.00 _cell_volume 697.03(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3605 _cell_measurement_theta_min 1 _cell_measurement_theta_max 37.04 _exptl_crystal_description 'plates' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.13 _exptl_crystal_density_diffrn 3.299 _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 5.330 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min 0.631 _exptl_absorpt_correction_T_max 0.863 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Kappa CCD' _diffrn_measurement_method 'omega-phi scans' _diffrn_reflns_number 2033 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 29.99 _reflns_number_total 2033 _reflns_number_observed 1883 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO (Otwinowski, 1997)' _computing_data_reduction 'SCALEPACK (Otwinowski, 1997)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 32 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.6144P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0041(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2001 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_obs 0.0259 _refine_ls_wR_factor_all 0.0692 _refine_ls_wR_factor_obs 0.0680 _refine_ls_goodness_of_fit_all 1.228 _refine_ls_goodness_of_fit_obs 1.253 _refine_ls_restrained_S_all 1.224 _refine_ls_restrained_S_obs 1.253 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn Zn 0.15008(4) 0.33834(4) 0.58506(4) 0.01041(11) Uani 1 d . . V V -0.43812(6) 0.00057(5) 0.74441(5) 0.00645(12) Uani 1 d . . P1 P -0.51063(8) 0.25154(8) 1.00164(7) 0.00588(14) Uani 1 d . . P2 P -0.03731(9) 0.12864(8) 0.77624(8) 0.0090(2) Uani 1 d . . Na Na -0.1928(2) 0.03019(15) 0.47822(14) 0.0165(3) Uani 1 d . . O1 O 0.0842(3) 0.1033(3) 0.8937(2) 0.0190(5) Uani 1 d . . O2 O -0.1544(2) -0.0008(2) 0.7625(2) 0.0101(4) Uani 1 d . . O3 O -0.4151(2) 0.1511(2) 0.9034(2) 0.0103(4) Uani 1 d . . O4 O -0.3933(2) 0.1607(2) 0.5986(2) 0.0093(4) Uani 1 d . . O5 O -0.3783(2) -0.1454(2) 0.5848(2) 0.0096(4) Uani 1 d . . O6 O -0.6233(3) -0.0162(3) 0.7299(2) 0.0154(4) Uani 1 d . . O7 O 0.0356(3) 0.1542(2) 0.6260(2) 0.0129(4) Uani 1 d . . O8 O -0.3816(2) -0.1590(2) 0.8965(2) 0.0090(4) Uani 1 d . . O9 O -0.1331(3) 0.2745(3) 0.8132(3) 0.0214(5) Uani 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 Zn 0.0105(2) 0.0107(2) 0.0100(2) -0.00012(12) -0.00194(12) -0.00152(12) V 0.0085(2) 0.0050(2) 0.0057(2) 0.00009(15) -0.0007(2) 0.0000(2) P1 0.0078(3) 0.0043(3) 0.0055(3) 0.0000(2) -0.0001(2) -0.0003(2) P2 0.0087(3) 0.0087(3) 0.0097(3) -0.0015(2) -0.0003(2) -0.0009(2) Na 0.0151(6) 0.0179(6) 0.0165(6) -0.0007(5) 0.0014(5) 0.0007(5) O1 0.0165(11) 0.0273(13) 0.0130(10) -0.0032(9) -0.0066(8) 0.0002(10) O2 0.0105(10) 0.0088(9) 0.0109(9) 0.0012(7) -0.0004(7) -0.0020(7) O3 0.0108(10) 0.0095(9) 0.0106(9) -0.0044(7) -0.0003(7) 0.0007(7) O4 0.0118(10) 0.0076(9) 0.0085(9) 0.0033(7) -0.0009(7) 0.0021(7) O5 0.0116(10) 0.0088(9) 0.0085(9) -0.0037(7) -0.0003(7) -0.0003(7) O6 0.0110(10) 0.0173(11) 0.0177(10) -0.0009(8) -0.0015(8) -0.0011(8) O7 0.0152(11) 0.0129(10) 0.0106(9) 0.0006(8) 0.0020(8) -0.0041(8) O8 0.0093(9) 0.0082(9) 0.0095(9) 0.0042(7) -0.0011(7) -0.0008(7) O9 0.0127(11) 0.0136(11) 0.0377(14) -0.0113(10) -0.0009(10) 0.0038(9) _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 Zn O1 1.889(2) 4_565 ? Zn O7 1.962(2) . ? Zn O8 1.981(2) 2_556 ? Zn O2 2.001(2) 2_556 ? Zn Na 3.3812(14) 3_556 ? V O6 1.592(2) . ? V O3 1.985(2) . ? V O4 1.998(2) . ? V O5 2.028(2) . ? V O8 2.042(2) . ? V O2 2.426(2) . ? V Na 3.2451(14) . ? P1 O3 1.519(2) . ? P1 O5 1.530(2) 2_456 ? P1 O4 1.538(2) 4_566 ? P1 O8 1.560(2) 3_457 ? P1 Na 3.360(2) 4_566 ? P2 O1 1.490(2) . ? P2 O7 1.530(2) . ? P2 O2 1.538(2) . ? P2 O9 1.585(2) . ? P2 Na 3.1176(15) . ? P2 Na 3.3824(15) 3_556 ? Na O7 2.345(3) 3_556 ? Na O4 2.364(2) . ? Na O9 2.370(3) 4_565 ? Na O6 2.435(3) 3_456 ? Na O5 2.450(2) . ? Na O7 2.596(3) . ? Na O2 2.611(2) . ? Na Na 3.354(3) 3_556 ? Na P1 3.3600(15) 4_565 ? Na Zn 3.3812(14) 3_556 ? O1 Zn 1.889(2) 4_566 ? O2 Zn 2.001(2) 2_546 ? O4 P1 1.538(2) 4_565 ? O5 P1 1.530(2) 2_446 ? O6 Na 2.435(3) 3_456 ? O7 Na 2.345(3) 3_556 ? O8 P1 1.560(2) 3_457 ? O8 Zn 1.981(2) 2_546 ? O9 Na 2.370(3) 4_566 ? 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 Zn O7 105.57(10) 4_565 . ? O1 Zn O8 110.58(10) 4_565 2_556 ? O7 Zn O8 119.66(9) . 2_556 ? O1 Zn O2 115.92(10) 4_565 2_556 ? O7 Zn O2 118.65(9) . 2_556 ? O8 Zn O2 85.95(8) 2_556 2_556 ? O1 Zn Na 98.40(8) 4_565 3_556 ? O7 Zn Na 42.49(7) . 3_556 ? O8 Zn Na 85.11(6) 2_556 3_556 ? O2 Zn Na 145.50(6) 2_556 3_556 ? O6 V O3 101.95(10) . . ? O6 V O4 102.57(10) . . ? O3 V O4 88.51(9) . . ? O6 V O5 98.34(10) . . ? O3 V O5 159.69(9) . . ? O4 V O5 86.38(8) . . ? O6 V O8 102.12(10) . . ? O3 V O8 88.17(8) . . ? O4 V O8 155.25(9) . . ? O5 V O8 88.29(8) . . ? O6 V O2 174.23(10) . . ? O3 V O2 82.59(8) . . ? O4 V O2 80.97(8) . . ? O5 V O2 77.20(8) . . ? O8 V O2 74.28(8) . . ? O6 V Na 127.09(9) . . ? O3 V Na 115.51(7) . . ? O4 V Na 46.45(6) . . ? O5 V Na 48.98(6) . . ? O8 V Na 114.48(7) . . ? O2 V Na 52.43(5) . . ? O3 P1 O5 113.14(12) . 2_456 ? O3 P1 O4 106.80(12) . 4_566 ? O5 P1 O4 111.90(12) 2_456 4_566 ? O3 P1 O8 111.35(12) . 3_457 ? O5 P1 O8 105.02(11) 2_456 3_457 ? O4 P1 O8 108.61(11) 4_566 3_457 ? O3 P1 Na 82.18(9) . 4_566 ? O5 P1 Na 96.16(9) 2_456 4_566 ? O4 P1 Na 38.68(8) 4_566 4_566 ? O8 P1 Na 146.83(8) 3_457 4_566 ? O1 P2 O7 111.77(13) . . ? O1 P2 O2 112.64(13) . . ? O7 P2 O2 108.54(12) . . ? O1 P2 O9 109.23(14) . . ? O7 P2 O9 106.69(14) . . ? O2 P2 O9 107.73(13) . . ? O1 P2 Na 148.84(11) . . ? O7 P2 Na 56.08(9) . . ? O2 P2 Na 56.67(8) . . ? O9 P2 Na 101.91(10) . . ? O1 P2 Na 91.07(10) . 3_556 ? O7 P2 Na 36.84(9) . 3_556 ? O2 P2 Na 90.71(9) . 3_556 ? O9 P2 Na 143.52(11) . 3_556 ? Na P2 Na 61.97(4) . 3_556 ? O7 Na O4 164.67(10) 3_556 . ? O7 Na O9 97.73(9) 3_556 4_565 ? O4 Na O9 95.37(9) . 4_565 ? O7 Na O6 90.89(9) 3_556 3_456 ? O4 Na O6 85.59(8) . 3_456 ? O9 Na O6 72.03(9) 4_565 3_456 ? O7 Na O5 94.93(8) 3_556 . ? O4 Na O5 69.81(8) . . ? O9 Na O5 151.18(10) 4_565 . ? O6 Na O5 82.02(8) 3_456 . ? O7 Na O7 94.66(8) 3_556 . ? O4 Na O7 95.28(8) . . ? O9 Na O7 80.78(9) 4_565 . ? O6 Na O7 152.74(9) 3_456 . ? O5 Na O7 123.89(8) . . ? O7 Na O2 105.26(8) 3_556 . ? O4 Na O2 70.85(7) . . ? O9 Na O2 132.87(10) 4_565 . ? O6 Na O2 145.83(9) 3_456 . ? O5 Na O2 66.99(7) . . ? O7 Na O2 57.14(7) . . ? O7 Na P2 108.30(7) 3_556 . ? O4 Na P2 75.93(6) . . ? O9 Na P2 104.22(8) 4_565 . ? O6 Na P2 160.81(8) 3_456 . ? O5 Na P2 96.13(6) . . ? O7 Na P2 29.28(5) . . ? O2 Na P2 29.48(5) . . ? O7 Na V 128.89(7) 3_556 . ? O4 Na V 37.77(5) . . ? O9 Na V 133.10(8) 4_565 . ? O6 Na V 99.09(7) 3_456 . ? O5 Na V 38.65(5) . . ? O7 Na V 98.06(6) . . ? O2 Na V 47.44(5) . . ? P2 Na V 69.28(3) . . ? O7 Na Na 50.48(6) 3_556 3_556 ? O4 Na Na 138.21(9) . 3_556 ? O9 Na Na 88.28(8) 4_565 3_556 ? O6 Na Na 134.34(9) 3_456 3_556 ? O5 Na Na 119.45(8) . 3_556 ? O7 Na Na 44.18(6) . 3_556 ? O2 Na Na 76.35(7) . 3_556 ? P2 Na Na 62.90(4) . 3_556 ? V Na Na 123.20(6) . 3_556 ? O7 Na P1 155.30(7) 3_556 4_565 ? O4 Na P1 23.99(5) . 4_565 ? O9 Na P1 78.08(7) 4_565 4_565 ? O6 Na P1 64.57(6) 3_456 4_565 ? O5 Na P1 79.62(6) . 4_565 ? O7 Na P1 108.45(7) . 4_565 ? O2 Na P1 94.82(6) . 4_565 ? P2 Na P1 96.27(4) . 4_565 ? V Na P1 57.63(3) . 4_565 ? Na Na P1 151.66(7) 3_556 4_565 ? O7 Na Zn 34.40(6) 3_556 3_556 ? O4 Na Zn 130.27(7) . 3_556 ? O9 Na Zn 126.28(8) 4_565 3_556 ? O6 Na Zn 83.54(6) 3_456 3_556 ? O5 Na Zn 60.67(6) . 3_556 ? O7 Na Zn 115.18(7) . 3_556 ? O2 Na Zn 92.98(6) . 3_556 ? P2 Na Zn 112.32(4) . 3_556 ? V Na Zn 96.90(4) . 3_556 ? Na Na Zn 75.66(5) 3_556 3_556 ? P1 Na Zn 132.26(4) 4_565 3_556 ? P2 O1 Zn 143.7(2) . 4_566 ? P2 O2 Zn 119.19(12) . 2_546 ? P2 O2 V 130.48(12) . . ? Zn O2 V 93.10(8) 2_546 . ? P2 O2 Na 93.85(10) . . ? Zn O2 Na 139.60(10) 2_546 . ? V O2 Na 80.13(7) . . ? P1 O3 V 141.79(14) . . ? P1 O4 V 128.10(13) 4_565 . ? P1 O4 Na 117.33(11) 4_565 . ? V O4 Na 95.78(8) . . ? P1 O5 V 126.51(13) 2_446 . ? P1 O5 Na 125.88(11) 2_446 . ? V O5 Na 92.37(8) . . ? V O6 Na 133.82(13) . 3_456 ? P2 O7 Zn 120.67(12) . . ? P2 O7 Na 120.14(12) . 3_556 ? Zn O7 Na 103.11(10) . 3_556 ? P2 O7 Na 94.64(11) . . ? Zn O7 Na 129.51(10) . . ? Na O7 Na 85.34(8) 3_556 . ? P1 O8 Zn 123.01(11) 3_457 2_546 ? P1 O8 V 129.90(12) 3_457 . ? Zn O8 V 106.67(9) 2_546 . ? P2 O9 Na 149.9(2) . 4_566 ? _refine_diff_density_max 0.655 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.131