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The novel title polyvanadate(V), poly[[octa-μ-aqua-dodeca­aqua-μ4-octa­cosa­oxidodeca­vanadato-hexa­sodium] tetra­hy­drate], [Na6(H2O)20(V10O28)·4H2O]n, contains [V10O28]6− anions which lie about inversion centres and have approximate 2/m symmetry and which are linked to [Na3(H2O)10]3+ cations through two terminal and two μ2-bridging O atoms. The structure contains three inequivalent Na+ cations, two of which form [Na2(H2O)8]n chains, which are linked via NaO6 octa­hedra involving the third Na+ ion, thus forming a three-dimensional framework.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270107025395/bc3048sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270107025395/bc3048Isup2.hkl
Contains datablock I

Comment top

Owing to their unusual topological properties and economically important applications in fields such as analytical chemistry, materials science and catalysis, nanotechnology, chemical sensing, luninescence, and medicine, polyoxometalates have aroused more and more attention in the past decade (Tanielian, 1998; Ouahab, 1998; Sadakane et al., 2000). Of the large polyoxometalate family, the most interesting class is polyoxovanadates, which are known to exhibit interesting physical and chemical properties with relevance to catalysis, biochemical processes and materials science (Zheng et al., 2005; Yang et al., 2003; Law et al., 2000). In recent years, a number of polyoxovanadate clusters exhibiting diverse topologies and interesting structural and electronic properties have been reported (Chen et al., 2005; Laye & McInnes, 2004). Although many compounds constructed from the [V10O28]6- polyoxoanion have been extensively studied, only a few complexes with three-dimensional frameworks have been reported (Zhang et al., 2004; Lee & Joo, 2003). In this communication, we describe a novel framework compound, Na6(H2O)20(V10O28)·4H2O, (I), prepared from V2O5, NaOH and HCl in solution.

The basic unit of (I) contains one [V10O28]6- polyanion with 2/m symmetry and two noncentrosymmetric [Na3(H2O)10]3+ cations (Fig. 1 and Table 1). The decavanadate anion is composed of ten VO6 octahedra combined via shared edges and shared corners. The bond lengths and angles of the [V10O28]6- anion are similar to those in the analogous compound Li6(H2O)16V10O28 (Xie & Ma, 2005). Bond valence sum calculations (Brown & Altermatt, 1985; O'Keeffe & Navrotsky, 1981) confirm that all the V atoms are in the +5 oxidation state (with bond valence sums in the 5.00–5.06 range).

There are three independent Na+ cations in (I). Atom Na1 is in a distorted octahedral coordination involving four O atoms (O20, O23, O24, O15B) from coordinated water molecules, one O atom (O1) from the [V10O28]6- anion and one µ2-O atom (O12B). Atoms Na2 and Na3 are both coordinated by six O atoms from water molecules that form distorted octahedral environments. Atoms Na2 and Na3 are linked by two µ2-O atoms (O16 and O18) to form dinuclear cations that are further linked to form [Na2(H2O)8]n chains in which the Na3···Na3A, Na2···Na2A and Na2···Na3 distances are 3.368 (3), 3.563 (3) and 3.448 (2) Å, respectively.

In the packing of (I), each [V10O28]6- anion acts as a µ4-bridge linking four Na1 cations through two terminal and two µ2-O atoms (Fig. 2). The decavanadate anions and the [Na2(H2O)8]n chains are linked to each other through Na1O6 octahedra to form a three-dimensional framework. To the best of our knowledge, a similar three-dimensional structure has not been described previously. In Na6V10O28.18H2O (Durif et al., 1980), decavanadate anions and trinuclear cations, [Na3(H2O)9]3+, link together to form a two-dimensional layer structure. In the related compound, K2Na4[V10O28].18H2O (Lee, 2006), chains of edge- and face-sharing [KO9] and [NaO6] polyhedra are interconnected by decavanadate anions to form a different three-dimensional network.

Related literature top

For related literature, see: Brown & Altermatt (1985); Chen et al. (2005); Durif et al. (1980); Law et al. (2000); Laye & McInnes (2004); Lee (2006); Lee & Joo (2003); O'Keeffe & Navrotsky (1981); Ouahab (1998); Sadakane et al. (2000); Tanielian (1998); Xie & Ma (2005); Yang et al. (2003); Zhang et al. (2004); Zheng et al. (2005).

Experimental top

The title compound was prepared by hydrothermal treatment of V2O5 (0.3861 g, 2.1 mmol) and NaOH (0.0672 g, 1.7 mmol) acidified to pH 5.8 with aqueous HCl. The reaction mixture was heated for 20 h at 393 K. The fitrate was kept at room temperature and block-shaped orange–yellow single crystals formed after one week. Compound (I) is air-stable both in the solid state and in solution at room temperature. The FT–IR spectrum of (I) shows two strong bands at 957 and 989 cm-1 that can be assigned to the stretching of the terminal V—O bonds. The antisymmetric modes of the V—O—V bridges possibly correspond to the bands at 750 and 848 cm-1, while the symmetric modes are probably at 558 and 605 cm-1. The broad band at 3467 cm-1 is due to the coordinated and solvent waters. Thermogravimetric analysis shows that the crystals lose 28.15 wt% in the temperature range 358–595 K. This is consistent with the number of coordinated and solvent water molecules in the molecular formula (28.28 wt%).

Refinement top

The coordinates of all H atoms were determined from a difference Fourier map. The H atoms were included in the final cycles of refinement with O—H and H···H distance restraints of 0.85 (1) and 1.39 (1) Å, respectively; Uiso(H) values were set at 1.5Ueq(O) for the coordinated water molecules and refined freely for the solvent molecules.

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1994); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The crystal structure of (I), showing 35% probability displacement ellipsoids. H atoms have been omitted for clarity.
[Figure 2] Fig. 2. Two-dimensional packing diagrams of (I) viewed along (a) the a axis and (b) the c axis.
poly[[octa-µ-aqua-dodecaaqua-µ-octacosaoxidodecavanadato-hexasodium] tetrahydrate] top
Crystal data top
Na6(H2O)20(V10O28)·4H2OZ = 1
Mr = 1527.72F(000) = 760
Triclinic, P1Dx = 2.249 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71070 Å
a = 10.5834 (3) ÅCell parameters from 4336 reflections
b = 11.3803 (3) Åθ = 3.1–25.4°
c = 11.6367 (3) ŵ = 2.16 mm1
α = 108.682 (4)°T = 223 K
β = 103.775 (2)°Block, orange-yellow
γ = 111.674 (3)°0.30 × 0.24 × 0.20 mm
V = 1128.19 (5) Å3
Data collection top
Siemens SMART CCD area-detector
diffractometer
4088 independent reflections
Radiation source: fine-focus sealed tube3529 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
ϕ and ω scansθmax = 25.4°, θmin = 3.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1211
Tmin = 0.542, Tmax = 0.649k = 1313
11109 measured reflectionsl = 1414
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.033H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.104 w = 1/[σ2(Fo2) + (0.070P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max = 0.001
4088 reflectionsΔρmax = 0.48 e Å3
379 parametersΔρmin = 0.46 e Å3
36 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0033 (8)
Crystal data top
Na6(H2O)20(V10O28)·4H2Oγ = 111.674 (3)°
Mr = 1527.72V = 1128.19 (5) Å3
Triclinic, P1Z = 1
a = 10.5834 (3) ÅMo Kα radiation
b = 11.3803 (3) ŵ = 2.16 mm1
c = 11.6367 (3) ÅT = 223 K
α = 108.682 (4)°0.30 × 0.24 × 0.20 mm
β = 103.775 (2)°
Data collection top
Siemens SMART CCD area-detector
diffractometer
4088 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
3529 reflections with I > 2σ(I)
Tmin = 0.542, Tmax = 0.649Rint = 0.028
11109 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03336 restraints
wR(F2) = 0.104H atoms treated by a mixture of independent and constrained refinement
S = 1.01Δρmax = 0.48 e Å3
4088 reflectionsΔρmin = 0.46 e Å3
379 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. 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 > σ(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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
V10.13667 (6)0.00678 (6)0.70287 (5)0.01648 (18)
V20.11146 (6)0.02394 (5)0.92289 (5)0.01133 (16)
V30.34146 (6)0.03813 (6)1.15233 (6)0.01602 (17)
V40.20972 (6)0.24151 (5)1.22011 (5)0.01235 (17)
V50.02637 (6)0.22625 (5)0.99442 (5)0.01259 (17)
Na10.19844 (16)0.09634 (15)0.39963 (15)0.0308 (4)
Na20.36612 (15)0.52124 (14)0.89519 (13)0.0235 (3)
Na30.11756 (14)0.50494 (13)0.62998 (13)0.0229 (3)
O10.1418 (3)0.0162 (3)0.5682 (2)0.0257 (6)
O20.0067 (2)0.1797 (2)0.8522 (2)0.0135 (5)
O30.0430 (3)0.3962 (2)1.0724 (2)0.0197 (5)
O40.3182 (2)0.0216 (2)1.2985 (2)0.0192 (5)
O50.1942 (2)0.1864 (2)1.3486 (2)0.0160 (5)
O60.2755 (3)0.4111 (2)1.2974 (2)0.0192 (5)
O70.1036 (2)0.0068 (2)1.0977 (2)0.0133 (5)
O80.3737 (2)0.2237 (2)1.2220 (2)0.0159 (5)
O90.5064 (3)0.0620 (2)1.1742 (2)0.0242 (6)
O100.0410 (2)0.1976 (2)0.8272 (2)0.0168 (5)
O110.1619 (2)0.2148 (2)1.0325 (2)0.0125 (5)
O120.0738 (2)0.0279 (2)0.7751 (2)0.0166 (5)
O130.2850 (2)0.0441 (2)0.9744 (2)0.0152 (5)
O140.2245 (2)0.1595 (2)0.9525 (2)0.0168 (5)
O150.1828 (3)0.7554 (3)0.7216 (2)0.0233 (6)
H15A0.126 (3)0.763 (4)0.762 (3)0.028*
H15B0.2723 (14)0.815 (3)0.776 (3)0.028*
O160.1082 (3)0.4662 (3)0.8234 (3)0.0251 (6)
H16B0.074 (4)0.389 (2)0.829 (4)0.030*
H16A0.080 (4)0.520 (3)0.868 (3)0.030*
O170.3951 (3)0.4729 (3)1.0801 (3)0.0259 (6)
H17A0.330 (3)0.3915 (15)1.062 (3)0.031*
H17B0.395 (4)0.536 (2)1.143 (3)0.031*
O180.3619 (3)0.5449 (3)0.6982 (3)0.0252 (6)
H18A0.375 (4)0.479 (2)0.652 (3)0.030*
H18B0.437 (3)0.6246 (17)0.724 (3)0.030*
O190.2325 (3)0.2764 (3)0.7523 (3)0.0274 (6)
H19A0.176 (3)0.235 (4)0.783 (4)0.033*
H19B0.284 (4)0.239 (4)0.734 (4)0.033*
O200.0561 (3)0.2605 (2)0.5176 (2)0.0229 (6)
H20A0.10460.25220.45560.027*
H20B0.09840.23420.58360.027*
O210.4387 (3)0.7589 (3)1.0145 (3)0.0276 (6)
H21A0.365 (2)0.774 (4)1.008 (4)0.033*
H21B0.509 (3)0.828 (3)1.017 (4)0.033*
O220.1307 (3)0.4616 (3)0.5609 (3)0.0265 (6)
H22A0.201 (3)0.3763 (14)0.525 (3)0.032*
H22B0.152 (4)0.515 (3)0.614 (3)0.032*
O230.3455 (3)0.1806 (3)0.4916 (3)0.0387 (7)
H23A0.339 (4)0.211 (4)0.5703 (14)0.046*
H23B0.4360 (19)0.139 (4)0.437 (3)0.046*
O240.3936 (3)0.1357 (3)0.2880 (3)0.0340 (7)
H24A0.439 (3)0.169 (4)0.329 (3)0.041*
H24B0.451 (3)0.168 (4)0.2079 (15)0.041*
O1W0.2809 (3)0.3030 (3)0.7664 (3)0.0340 (7)
H1WA0.261 (5)0.245 (3)0.787 (4)0.061 (17)*
H1WB0.212 (4)0.3870 (16)0.817 (4)0.058 (16)*
O2W0.4468 (3)0.3331 (3)1.5892 (3)0.0333 (7)
H2WA0.387 (3)0.297 (4)1.5090 (17)0.043 (13)*
H2WB0.5351 (17)0.378 (5)1.598 (4)0.077 (19)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.0162 (3)0.0168 (3)0.0144 (3)0.0054 (3)0.0051 (2)0.0085 (2)
V20.0107 (3)0.0106 (3)0.0125 (3)0.0042 (2)0.0062 (2)0.0051 (2)
V30.0109 (3)0.0156 (3)0.0198 (3)0.0055 (2)0.0053 (2)0.0078 (3)
V40.0114 (3)0.0097 (3)0.0115 (3)0.0026 (2)0.0038 (2)0.0034 (2)
V50.0117 (3)0.0097 (3)0.0155 (3)0.0049 (2)0.0049 (2)0.0055 (2)
Na10.0305 (8)0.0241 (8)0.0307 (8)0.0068 (7)0.0096 (7)0.0140 (7)
Na20.0222 (7)0.0212 (7)0.0259 (8)0.0089 (6)0.0081 (6)0.0122 (6)
Na30.0218 (8)0.0234 (8)0.0255 (8)0.0120 (6)0.0101 (6)0.0117 (6)
O10.0289 (14)0.0281 (14)0.0175 (13)0.0091 (12)0.0077 (11)0.0142 (11)
O20.0126 (11)0.0102 (11)0.0159 (12)0.0045 (9)0.0069 (9)0.0044 (9)
O30.0205 (13)0.0097 (11)0.0269 (13)0.0064 (10)0.0091 (11)0.0075 (10)
O40.0161 (12)0.0181 (12)0.0193 (12)0.0053 (10)0.0030 (10)0.0105 (10)
O50.0158 (12)0.0150 (12)0.0126 (11)0.0044 (10)0.0053 (9)0.0050 (9)
O60.0189 (12)0.0127 (12)0.0197 (12)0.0043 (10)0.0078 (10)0.0041 (10)
O70.0099 (11)0.0133 (12)0.0149 (12)0.0043 (10)0.0041 (9)0.0068 (10)
O80.0119 (11)0.0134 (12)0.0184 (12)0.0038 (9)0.0040 (10)0.0068 (10)
O90.0141 (12)0.0233 (13)0.0306 (14)0.0085 (11)0.0068 (11)0.0093 (11)
O100.0160 (12)0.0151 (12)0.0199 (12)0.0055 (10)0.0071 (10)0.0110 (10)
O110.0111 (11)0.0111 (11)0.0134 (11)0.0035 (9)0.0049 (9)0.0055 (9)
O120.0162 (12)0.0161 (12)0.0147 (12)0.0038 (10)0.0077 (10)0.0076 (10)
O130.0132 (12)0.0125 (11)0.0178 (12)0.0045 (9)0.0081 (10)0.0052 (9)
O140.0130 (11)0.0148 (12)0.0223 (13)0.0077 (10)0.0068 (10)0.0070 (10)
O150.0176 (13)0.0226 (14)0.0222 (13)0.0066 (11)0.0081 (11)0.0053 (11)
O160.0286 (14)0.0253 (14)0.0355 (15)0.0169 (12)0.0216 (12)0.0188 (12)
O170.0230 (14)0.0236 (14)0.0276 (15)0.0059 (12)0.0131 (12)0.0118 (12)
O180.0175 (13)0.0175 (13)0.0311 (15)0.0028 (11)0.0079 (11)0.0086 (12)
O190.0239 (15)0.0217 (14)0.0384 (16)0.0092 (12)0.0156 (12)0.0155 (12)
O200.0259 (14)0.0230 (13)0.0230 (13)0.0125 (11)0.0122 (11)0.0114 (11)
O210.0216 (14)0.0191 (14)0.0412 (16)0.0084 (11)0.0186 (13)0.0102 (12)
O220.0255 (14)0.0256 (14)0.0294 (15)0.0127 (12)0.0135 (12)0.0117 (12)
O230.0327 (16)0.0407 (17)0.0342 (16)0.0131 (14)0.0134 (13)0.0131 (14)
O240.0271 (15)0.0320 (16)0.0362 (16)0.0095 (13)0.0093 (13)0.0162 (14)
O1W0.0244 (15)0.0340 (17)0.0385 (17)0.0107 (14)0.0067 (13)0.0190 (15)
O2W0.0217 (15)0.0347 (16)0.0259 (16)0.0037 (13)0.0022 (12)0.0111 (13)
Geometric parameters (Å, º) top
V1—O11.594 (2)Na2—O172.366 (3)
V1—O4i1.822 (2)Na2—O182.385 (3)
V1—O101.870 (2)Na2—O162.420 (3)
V1—O5i1.886 (2)Na2—O17iv2.448 (3)
V1—O122.076 (2)Na2—Na33.4475 (18)
V1—O7i2.327 (2)Na2—Na2iv3.562 (3)
V1—V3i3.0447 (8)Na2—H16B2.67 (3)
V1—V23.0965 (7)Na3—O182.334 (3)
V1—V53.1053 (8)Na3—O222.361 (3)
V1—V4i3.1184 (7)Na3—O22ii2.397 (3)
V2—O121.689 (2)Na3—O202.408 (3)
V2—O131.692 (2)Na3—O162.445 (3)
V2—O111.917 (2)Na3—O152.447 (3)
V2—O21.930 (2)Na3—Na3ii3.369 (3)
V2—O7i2.112 (2)O2—V4i1.991 (2)
V2—O72.123 (2)O2—V5i2.005 (2)
V2—V33.0689 (7)O4—V1i1.822 (2)
V3—O91.606 (2)O5—V1i1.886 (2)
V3—O41.833 (2)O7—V2i2.112 (2)
V3—O81.864 (2)O7—V5i2.239 (2)
V3—O14i1.883 (2)O7—V1i2.327 (2)
V3—O132.044 (2)O12—Na1iii2.948 (3)
V3—O72.301 (2)O14—V3i1.883 (2)
V3—V1i3.0447 (8)O15—Na1ii2.508 (3)
V3—V43.1082 (8)O15—H15A0.857 (11)
V3—V5i3.1103 (8)O15—H15B0.849 (11)
V4—O61.617 (2)O16—H16B0.853 (11)
V4—O51.816 (2)O16—H16A0.855 (11)
V4—O81.816 (2)O17—Na2iv2.448 (3)
V4—O2i1.991 (2)O17—H17A0.843 (11)
V4—O112.013 (2)O17—H17B0.845 (11)
V4—O72.238 (2)O18—H18A0.849 (11)
V4—V53.0713 (7)O18—H18B0.852 (11)
V4—V1i3.1184 (7)O19—H19A0.842 (11)
V5—O31.617 (2)O19—H19B0.840 (11)
V5—O141.820 (2)O20—H20A0.9800
V5—O101.825 (2)O20—H20B0.9800
V5—O111.998 (2)O21—H21A0.855 (11)
V5—O2i2.005 (2)O21—H21B0.848 (11)
V5—O7i2.239 (2)O22—Na3ii2.397 (3)
V5—V3i3.1103 (8)O22—H22A0.854 (11)
Na1—O242.328 (3)O22—H22B0.850 (11)
Na1—O202.348 (3)O23—H23A0.844 (11)
Na1—O232.393 (3)O23—H23B0.851 (11)
Na1—O12.455 (3)O24—H24A0.833 (11)
Na1—O15ii2.508 (3)O24—H24B0.846 (11)
Na1—O12iii2.948 (3)O1W—H1WA0.845 (11)
Na1—Na34.0313 (19)O1W—H1WB0.843 (11)
Na2—O212.320 (3)O2W—H2WA0.848 (11)
Na2—O192.352 (3)O2W—H2WB0.846 (11)
O1—V1—O4i104.20 (12)O3—V5—V3i136.82 (9)
O1—V1—O10102.55 (12)O14—V5—V3i33.50 (7)
O4i—V1—O1093.04 (10)O10—V5—V3i84.08 (7)
O1—V1—O5i101.57 (12)O11—V5—V3i123.59 (6)
O4i—V1—O5i91.57 (10)O2i—V5—V3i86.66 (6)
O10—V1—O5i153.49 (10)O7i—V5—V3i47.61 (5)
O1—V1—O1299.81 (12)V4—V5—V3i118.93 (2)
O4i—V1—O12155.93 (10)V1—V5—V3i58.662 (18)
O10—V1—O1283.34 (10)O24—Na1—O20151.00 (12)
O5i—V1—O1281.88 (9)O24—Na1—O2391.49 (11)
O1—V1—O7i173.52 (11)O20—Na1—O23111.43 (11)
O4i—V1—O7i82.22 (9)O24—Na1—O180.53 (10)
O10—V1—O7i77.66 (8)O20—Na1—O181.30 (9)
O5i—V1—O7i77.13 (8)O23—Na1—O191.56 (11)
O12—V1—O7i73.74 (8)O24—Na1—O15ii116.97 (11)
O1—V1—V3i137.92 (10)O20—Na1—O15ii82.00 (9)
O4i—V1—V3i33.72 (7)O23—Na1—O15ii89.50 (11)
O10—V1—V3i85.29 (7)O1—Na1—O15ii162.44 (10)
O5i—V1—V3i84.18 (7)O24—Na1—O12iii81.98 (10)
O12—V1—V3i122.24 (6)O20—Na1—O12iii78.92 (8)
O7i—V1—V3i48.50 (5)O23—Na1—O12iii166.07 (11)
O1—V1—V2130.58 (10)O1—Na1—O12iii99.43 (9)
O4i—V1—V2125.20 (7)O15ii—Na1—O12iii82.62 (8)
O10—V1—V277.90 (7)O24—Na1—Na3172.40 (10)
O5i—V1—V278.13 (7)O20—Na1—Na332.51 (6)
O12—V1—V230.78 (6)O23—Na1—Na382.04 (8)
O7i—V1—V242.98 (5)O1—Na1—Na395.58 (7)
V3i—V1—V291.48 (2)O15ii—Na1—Na367.20 (7)
O1—V1—V5134.84 (9)O12iii—Na1—Na3105.18 (6)
O4i—V1—V582.61 (7)O21—Na2—O19165.24 (11)
O10—V1—V532.38 (7)O21—Na2—O1795.54 (10)
O5i—V1—V5123.09 (7)O19—Na2—O1789.78 (10)
O12—V1—V581.72 (6)O21—Na2—O1892.29 (10)
O7i—V1—V545.96 (5)O19—Na2—O1884.58 (10)
V3i—V1—V560.752 (18)O17—Na2—O18168.83 (11)
V2—V1—V561.152 (17)O21—Na2—O1689.89 (10)
O1—V1—V4i133.45 (9)O19—Na2—O1675.59 (10)
O4i—V1—V4i82.22 (7)O17—Na2—O16100.36 (10)
O10—V1—V4i123.38 (7)O18—Na2—O1687.59 (9)
O5i—V1—V4i31.92 (7)O21—Na2—O17iv102.08 (10)
O12—V1—V4i80.05 (6)O19—Na2—O17iv92.11 (10)
O7i—V1—V4i45.74 (5)O17—Na2—O17iv84.54 (9)
V3i—V1—V4i60.559 (17)O18—Na2—O17iv86.04 (9)
V2—V1—V4i61.003 (17)O16—Na2—O17iv166.64 (11)
V5—V1—V4i91.531 (19)O21—Na2—Na389.55 (8)
O12—V2—O13106.75 (11)O19—Na2—Na378.39 (8)
O12—V2—O1198.51 (10)O17—Na2—Na3145.26 (8)
O13—V2—O1197.46 (10)O18—Na2—Na342.49 (7)
O12—V2—O296.48 (10)O16—Na2—Na345.17 (7)
O13—V2—O296.51 (10)O17iv—Na2—Na3127.95 (8)
O11—V2—O2155.60 (10)O21—Na2—Na2iv102.00 (9)
O12—V2—O7i87.65 (10)O19—Na2—Na2iv91.30 (8)
O13—V2—O7i165.57 (10)O17—Na2—Na2iv43.16 (7)
O11—V2—O7i80.82 (9)O18—Na2—Na2iv127.16 (9)
O2—V2—O7i80.67 (9)O16—Na2—Na2iv142.00 (9)
O12—V2—O7165.93 (10)O17iv—Na2—Na2iv41.38 (6)
O13—V2—O787.24 (9)Na3—Na2—Na2iv165.53 (7)
O11—V2—O780.64 (9)O21—Na2—H16B104.0 (5)
O2—V2—O780.16 (9)O19—Na2—H16B62.4 (5)
O7i—V2—O778.33 (9)O17—Na2—H16B87.1 (6)
O12—V2—V3145.46 (8)O18—Na2—H16B98.8 (7)
O13—V2—V338.71 (7)O16—Na2—H16B18.5 (4)
O11—V2—V389.34 (7)O17iv—Na2—H16B153.2 (4)
O2—V2—V389.14 (7)Na3—Na2—H16B58.4 (6)
O7i—V2—V3126.87 (6)Na2iv—Na2—H16B125.4 (5)
O7—V2—V348.53 (6)O18—Na3—O22179.26 (10)
O12—V2—V138.97 (8)O18—Na3—O22ii90.51 (10)
O13—V2—V1145.72 (8)O22—Na3—O22ii89.86 (9)
O11—V2—V189.63 (7)O18—Na3—O2083.78 (9)
O2—V2—V190.01 (7)O22—Na3—O2095.57 (10)
O7i—V2—V148.70 (6)O22ii—Na3—O2091.32 (9)
O7—V2—V1127.03 (6)O18—Na3—O1688.14 (10)
V3—V2—V1175.57 (2)O22—Na3—O1691.48 (10)
O9—V3—O4104.26 (12)O22ii—Na3—O16178.15 (10)
O9—V3—O8101.96 (11)O20—Na3—O1687.28 (9)
O4—V3—O891.34 (10)O18—Na3—O1595.80 (10)
O9—V3—O14i102.14 (11)O22—Na3—O1584.88 (9)
O4—V3—O14i90.92 (10)O22ii—Na3—O1582.17 (9)
O8—V3—O14i154.43 (10)O20—Na3—O15173.48 (10)
O9—V3—O1398.12 (11)O16—Na3—O1599.22 (10)
O4—V3—O13157.62 (10)O18—Na3—Na3ii135.00 (10)
O8—V3—O1384.21 (9)O22—Na3—Na3ii45.36 (7)
O14i—V3—O1384.06 (10)O22ii—Na3—Na3ii44.50 (7)
O9—V3—O7173.01 (11)O20—Na3—Na3ii94.84 (8)
O4—V3—O782.72 (9)O16—Na3—Na3ii136.83 (9)
O8—V3—O777.32 (9)O15—Na3—Na3ii80.83 (8)
O14i—V3—O777.71 (9)O18—Na3—Na243.64 (7)
O13—V3—O774.90 (8)O22—Na3—Na2136.01 (8)
O9—V3—V1i137.75 (9)O22ii—Na3—Na2134.12 (8)
O4—V3—V1i33.49 (7)O20—Na3—Na285.78 (7)
O8—V3—V1i84.17 (7)O16—Na3—Na244.58 (7)
O14i—V3—V1i83.76 (7)O15—Na3—Na298.43 (7)
O13—V3—V1i124.13 (7)Na3ii—Na3—Na2178.46 (7)
O7—V3—V1i49.23 (5)O18—Na3—Na1115.37 (8)
O9—V3—V2129.30 (9)O22—Na3—Na163.98 (7)
O4—V3—V2126.44 (8)O22ii—Na3—Na191.39 (7)
O8—V3—V278.73 (7)O20—Na3—Na131.59 (6)
O14i—V3—V279.47 (7)O16—Na3—Na188.05 (7)
O13—V3—V231.19 (6)O15—Na3—Na1148.28 (8)
O7—V3—V243.72 (5)Na3ii—Na3—Na173.13 (5)
V1i—V3—V292.95 (2)Na2—Na3—Na1107.99 (4)
O9—V3—V4133.83 (9)V1—O1—Na1154.17 (16)
O4—V3—V482.35 (7)V2—O2—V4i107.13 (10)
O8—V3—V431.89 (7)V2—O2—V5i107.89 (10)
O14i—V3—V4123.65 (7)V4i—O2—V5i100.48 (10)
O13—V3—V482.37 (6)V1i—O4—V3112.79 (12)
O7—V3—V445.95 (5)V4—O5—V1i114.77 (12)
V1i—V3—V460.892 (17)V2i—O7—V2101.67 (9)
V2—V3—V461.834 (17)V2i—O7—V492.92 (8)
O9—V3—V5i134.37 (9)V2—O7—V493.37 (8)
O4—V3—V5i82.31 (7)V2i—O7—V5i92.92 (8)
O8—V3—V5i123.24 (7)V2—O7—V5i93.63 (8)
O14i—V3—V5i32.24 (7)V4—O7—V5i169.80 (11)
O13—V3—V5i81.88 (6)V2i—O7—V3170.58 (11)
O7—V3—V5i45.92 (5)V2—O7—V387.75 (8)
V1i—V3—V5i60.586 (18)V4—O7—V386.41 (7)
V2—V3—V5i61.960 (17)V5i—O7—V386.47 (7)
V4—V3—V5i91.63 (2)V2i—O7—V1i88.32 (8)
O6—V4—O5102.96 (11)V2—O7—V1i170.01 (11)
O6—V4—O8103.35 (11)V4—O7—V1i86.14 (7)
O5—V4—O894.37 (10)V5i—O7—V1i85.68 (7)
O6—V4—O2i99.70 (11)V3—O7—V1i82.26 (7)
O5—V4—O2i91.01 (10)V4—O8—V3115.28 (11)
O8—V4—O2i154.46 (10)V5—O10—V1114.34 (11)
O6—V4—O1199.82 (10)V2—O11—V5107.38 (10)
O5—V4—O11155.46 (10)V2—O11—V4107.72 (10)
O8—V4—O1189.10 (10)V5—O11—V499.95 (10)
O2i—V4—O1176.19 (9)V2—O12—V1110.25 (12)
O6—V4—O7174.61 (10)V2—O12—Na1iii117.19 (11)
O5—V4—O780.88 (9)V1—O12—Na1iii122.48 (10)
O8—V4—O779.94 (9)V2—O13—V3110.10 (11)
O2i—V4—O776.30 (8)V5—O14—V3i114.26 (11)
O11—V4—O775.82 (8)Na3—O15—Na1ii127.26 (11)
O6—V4—V589.61 (9)Na3—O15—H15A105 (2)
O5—V4—V5130.93 (7)Na1ii—O15—H15A109 (3)
O8—V4—V5128.94 (7)Na3—O15—H15B117 (2)
O2i—V4—V539.92 (6)Na1ii—O15—H15B89 (3)
O11—V4—V539.84 (6)H15A—O15—H15B108.4 (17)
O7—V4—V585.01 (6)Na2—O16—Na390.25 (9)
O6—V4—V3136.03 (9)Na2—O16—H16B97 (2)
O5—V4—V383.41 (7)Na3—O16—H16B130 (2)
O8—V4—V332.83 (7)Na2—O16—H16A122 (3)
O2i—V4—V3123.89 (7)Na3—O16—H16A110 (2)
O11—V4—V386.53 (6)H16B—O16—H16A107.9 (17)
O7—V4—V347.65 (6)Na2—O17—Na2iv95.46 (9)
V5—V4—V3119.11 (2)Na2—O17—H17A113 (3)
O6—V4—V1i136.07 (9)Na2iv—O17—H17A110 (2)
O5—V4—V1i33.31 (7)Na2—O17—H17B110 (3)
O8—V4—V1i82.74 (7)Na2iv—O17—H17B117 (3)
O2i—V4—V1i88.28 (6)H17A—O17—H17B110.5 (18)
O11—V4—V1i123.94 (6)Na3—O18—Na293.87 (10)
O7—V4—V1i48.13 (6)Na3—O18—H18A116 (2)
V5—V4—V1i120.53 (2)Na2—O18—H18A106 (3)
V3—V4—V1i58.548 (18)Na3—O18—H18B123 (2)
O3—V5—O14103.46 (11)Na2—O18—H18B106 (3)
O3—V5—O10102.49 (11)H18A—O18—H18B109.1 (18)
O14—V5—O1094.98 (10)Na2—O19—H19A109 (3)
O3—V5—O1199.28 (11)Na2—O19—H19B115 (3)
O14—V5—O11155.10 (10)H19A—O19—H19B111.9 (19)
O10—V5—O1189.86 (10)Na1—O20—Na3115.90 (11)
O3—V5—O2i100.05 (11)Na1—O20—H20A108.3
O14—V5—O2i89.83 (10)Na3—O20—H20A108.3
O10—V5—O2i155.14 (10)Na1—O20—H20B108.3
O11—V5—O2i76.22 (9)Na3—O20—H20B108.3
O3—V5—O7i174.28 (10)H20A—O20—H20B107.4
O14—V5—O7i80.64 (9)Na2—O21—H21A112 (2)
O10—V5—O7i80.94 (9)Na2—O21—H21B126 (2)
O11—V5—O7i76.02 (8)H21A—O21—H21B108.5 (17)
O2i—V5—O7i75.80 (8)Na3—O22—Na3ii90.14 (9)
O3—V5—V489.49 (8)Na3—O22—H22A119 (2)
O14—V5—V4129.43 (7)Na3ii—O22—H22A102 (2)
O10—V5—V4130.06 (7)Na3—O22—H22B118 (2)
O11—V5—V440.20 (6)Na3ii—O22—H22B118 (3)
O2i—V5—V439.60 (6)H22A—O22—H22B108.7 (18)
O7i—V5—V484.82 (6)Na1—O23—H23A130 (3)
O3—V5—V1135.54 (9)Na1—O23—H23B113 (3)
O14—V5—V182.96 (7)H23A—O23—H23B109.8 (18)
O10—V5—V133.29 (7)Na1—O24—H24A119 (3)
O11—V5—V187.93 (6)Na1—O24—H24B120 (2)
O2i—V5—V1124.15 (6)H24A—O24—H24B111.5 (19)
O7i—V5—V148.36 (6)H1WA—O1W—H1WB110.6 (19)
V4—V5—V1120.52 (2)H2WA—O2W—H2WB109.5 (19)
Symmetry codes: (i) x, y, z+2; (ii) x, y+1, z+1; (iii) x, y, z+1; (iv) x+1, y+1, z+2.

Experimental details

Crystal data
Chemical formulaNa6(H2O)20(V10O28)·4H2O
Mr1527.72
Crystal system, space groupTriclinic, P1
Temperature (K)223
a, b, c (Å)10.5834 (3), 11.3803 (3), 11.6367 (3)
α, β, γ (°)108.682 (4), 103.775 (2), 111.674 (3)
V3)1128.19 (5)
Z1
Radiation typeMo Kα
µ (mm1)2.16
Crystal size (mm)0.30 × 0.24 × 0.20
Data collection
DiffractometerSiemens SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.542, 0.649
No. of measured, independent and
observed [I > 2σ(I)] reflections
11109, 4088, 3529
Rint0.028
(sin θ/λ)max1)0.602
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.033, 0.104, 1.01
No. of reflections4088
No. of parameters379
No. of restraints36
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.48, 0.46

Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1994), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1997), SHELXL97.

Selected geometric parameters (Å, º) top
V1—O11.594 (2)Na1—O232.393 (3)
V1—O4i1.822 (2)Na1—O12.455 (3)
V1—O5i1.886 (2)Na1—O15ii2.508 (3)
V2—O121.689 (2)Na1—O12iii2.948 (3)
V2—O7i2.112 (2)Na2—O212.320 (3)
V3—O91.606 (2)Na2—O192.352 (3)
V4—O51.816 (2)Na2—O162.420 (3)
V5—O141.820 (2)Na3—O182.334 (3)
Na1—O242.328 (3)Na3—O22ii2.397 (3)
Na1—O202.348 (3)Na3—O162.445 (3)
O1—V1—O4i104.20 (12)O24—Na1—O12iii81.98 (10)
O1—V1—O10102.55 (12)O23—Na1—O12iii166.07 (11)
O4i—V1—O5i91.57 (10)O15ii—Na1—O12iii82.62 (8)
O4i—V1—O12155.93 (10)O19—Na2—O1884.58 (10)
O5i—V1—O1281.88 (9)O21—Na2—O1689.89 (10)
O5i—V1—O7i77.13 (8)O17—Na2—O16100.36 (10)
O24—Na1—O20151.00 (12)O19—Na2—O17iv92.11 (10)
O20—Na1—O23111.43 (11)O16—Na2—O17iv166.64 (11)
O20—Na1—O181.30 (9)O22ii—Na3—O2091.32 (9)
O23—Na1—O191.56 (11)O22ii—Na3—O16178.15 (10)
O20—Na1—O15ii82.00 (9)O18—Na3—O1595.80 (10)
O23—Na1—O15ii89.50 (11)
Symmetry codes: (i) x, y, z+2; (ii) x, y+1, z+1; (iii) x, y, z+1; (iv) x+1, y+1, z+2.
 

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