(NH4)4Na2[V10O28]·10H2O

Fratzky, D.; Schneider, M.; Rabe, S.; Meisel, M.

doi:10.1107/S0108270100005448

(NH₄)₄Na₂[V₁₀O₂₈]·10H₂O

D. Fratzky, M. Schneider, S. Rabe and M. Meisel

Tetraammonium disodium decavanadate decahydrate crystallizes in the triclinic system in space group P $\overline 1$ . The structure contains typical centrosymmetric OV₆ double octahedra and centrosymmetric pairs of edge-shared NaO₆ double octahedra forming a layered structure. In contrast to other monovalent cationic decavanadates, the NaO₆ double octahedra are integrated in the layer.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100005448/br1283sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S0108270100005448/br1283Isup2.hkl Contains datablock I

Comment top

Vanadium compounds, particularly vanadium phosphates, are of great interest as potential catalysts for heterogeneous oxidation and ammoxidation reactions (Centi, 1993). In connection with the investigation of the system NH₃–V^V, we found the decavanadate (NH₄)₄Na₂(V₁₀O₂₈)^.10H₂O, (I), and determined its crystal structure. (I) crystallizes during very slow evaporation of an appropriate solution. There exist several structures of monovalent cation decavanadates of the type M_x(V₁₀O₂₈)^.yH₂O. Thus, crystal structures are known from Na₆(V₁₀O₂₈)^.18H₂O (Durif et al., 1982), Na₆(V₁₀O₂₈)^.12H₂O (Xu et al., 1996), Cs₄H₂(V₁₀O₂₈)^.4H₂O (Rigotti et al., 1987) and (NH₄)₆(V₁₀O₂₈)^.6H₂O (Eglmeier et al., 1993). The structure of (I) consists of layers of decavanadate anions and pairs of edge-shared NaO₆ double octahedra (Fig. 1). The layered structure is similar to those found for the other decavanadates of monovalent cations, but in (I), the layers are connected only via hydrogen bonds. This is unusual because in the other decavanadates mentioned above, the layers are connected via cation polyhedra. However, in the present structure all NaO₆ octahedra are integrated in the layer.

The [V₁₀O₂₈]⁶⁻ decavanadate anions appear as common edge-shared OV₆ double octahedra. The axial V—O bond distances are in the normal ranges, with values of 1.60–1.69 Å for the V═O group and of 2.10–2.35 Å for the second axial O atom, as are the four equatorial V—O bonds with distances ranging from 1.70 to 2.09 Å. Sodium occurs as a pair of edge-shared NaO₆ octahedra. In the octahedron, sodium is surrounded by six water molecules, the only water in the structure. The Na—O bond distances are in the narrow range 2.34–2.44 Å. In the above-mentioned sodium decavanadates, longer Na—O distances were found (up to 2.7 Å). The H atoms of the coordinated water are involved in hydrogen bridges, forming the linkage between the decavanadate anions in the layer as well as forming bridges to neighbouring layers.

The N1 and N2 ammonium ions are fixed via hydrogen bonds to the decavanadate anion. Additionally, they form hydrogen bonds to the sodium–oxygen octahedron and to one decavanadate anion of a neighbouring layer. Compound (I) is a new decavanadate with some interesting structural features, especially with regard to the arrangement of the layers, which is quite different from what is found in other decavanadates of monovalent cations.

Experimental top

(NH₄)₄Na₂(V₁₀O₂₈)^.10H₂O was prepared by evaporation of a solution consisting of H₂O (50 ml), NH₄VO₃ (250 mg) and NaH₂PO₄ (50 mg) at room temperature.

Computing details top

Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: CORINC (Schollmeyer, 1992); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Bergerhoff, 1996); software used to prepare material for publication: SHELXL97.

Figures top

	Fig. 1. View along the a axis showing the edge-shared NaO₆ double octahedra (light grey).
	Fig. 2. A plot with displacement ellipsoids of the [V₁₀O₂₈]⁶⁻ anion drawn at the 50% probability level; V atoms are shaded.

Tetraammonium dinatrium decavanadate 10-hydrate top

Crystal data top

(NH₄)₄[Na₂(H₂O)₁₀][V₁₀O₂₈]	Z = 1
M_r = 1255.71	F(000) = 620
Triclinic, P1	D_x = 2.448 Mg m⁻³
a = 8.501 (2) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.426 (2) Å	Cell parameters from 25 reflections
c = 11.282 (2) Å	θ = 10–18°
α = 68.46 (3)°	µ = 2.77 mm⁻¹
β = 87.30 (3)°	T = 293 K
γ = 67.14 (3)°	Plate, red
V = 851.7 (3) Å³	0.2 × 0.2 × 0.1 mm

Data collection top

Enraf-Nonius CAD-4 diffractometer	4474 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.007
Graphite monochromator	θ_max = 30.0°, θ_min = 2.0°
θ/2θ scans	h = 0→11
Absorption correction: ψ scan (CORINC; Schollmeyer, 1992)	k = −13→14
T_min = 0.632, T_max = 0.758	l = −15→15
5282 measured reflections	3 standard reflections every 100 reflections
4933 independent reflections	intensity decay: none

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.102	All H-atom parameters refined
S = 1.06	Calculated w = 1/[σ²(F_o²) + (0.0727P)² + 0.331P] where P = (F_o² + 2F_c²)/3
4933 reflections	(Δ/σ)_max = 0.005
316 parameters	Δρ_max = 1.31 e Å⁻³
0 restraints	Δρ_min = −1.17 e Å⁻³

Crystal data top

(NH₄)₄[Na₂(H₂O)₁₀][V₁₀O₂₈]	γ = 67.14 (3)°
M_r = 1255.71	V = 851.7 (3) Å³
Triclinic, P1	Z = 1
a = 8.501 (2) Å	Mo Kα radiation
b = 10.426 (2) Å	µ = 2.77 mm⁻¹
c = 11.282 (2) Å	T = 293 K
α = 68.46 (3)°	0.2 × 0.2 × 0.1 mm
β = 87.30 (3)°

Data collection top

Enraf-Nonius CAD-4 diffractometer	4474 reflections with I > 2σ(I)
Absorption correction: ψ scan (CORINC; Schollmeyer, 1992)	R_int = 0.007
T_min = 0.632, T_max = 0.758	3 standard reflections every 100 reflections
5282 measured reflections	intensity decay: none
4933 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.036	0 restraints
wR(F²) = 0.102	All H-atom parameters refined
S = 1.06	Δρ_max = 1.31 e Å⁻³
4933 reflections	Δρ_min = −1.17 e Å⁻³
316 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

	x	y	z	U_iso*/U_eq
V1	0.03006 (4)	0.29101 (4)	0.23781 (3)	0.01885 (9)
V2	0.19030 (4)	0.00256 (3)	0.48069 (3)	0.01351 (8)
V3	−0.02605 (4)	0.00443 (3)	0.26033 (3)	0.01707 (9)
V4	0.12336 (4)	−0.28293 (3)	0.50328 (3)	0.01748 (9)
V5	0.32808 (4)	−0.28412 (4)	0.72318 (3)	0.01970 (9)
Na	0.56828 (12)	−0.16738 (10)	0.12645 (9)	0.0318 (2)
O1	0.23957 (17)	0.13239 (15)	0.35981 (13)	0.0186 (3)
O2	−0.06686 (15)	0.12408 (14)	0.39460 (12)	0.0153 (2)
O3	0.06164 (18)	0.14112 (15)	0.17219 (13)	0.0194 (3)
O4	−0.01624 (18)	0.36875 (15)	0.36709 (13)	0.0198 (3)
O5	0.1116 (2)	0.39637 (18)	0.13910 (15)	0.0287 (3)
O6	0.20098 (18)	−0.38051 (15)	0.82265 (13)	0.0212 (3)
O7	0.37517 (17)	−0.12154 (15)	0.57503 (13)	0.0194 (3)
O8	0.10344 (16)	0.12031 (14)	0.58412 (12)	0.0159 (2)
O9	0.18432 (16)	−0.11584 (14)	0.38562 (12)	0.0162 (2)
O10	0.0084 (2)	−0.09796 (17)	0.17518 (14)	0.0253 (3)
O11	0.24871 (17)	−0.13473 (15)	0.79406 (13)	0.0196 (3)
O12	0.1573 (2)	−0.38177 (16)	0.41571 (15)	0.0260 (3)
O13	0.32924 (17)	−0.36407 (15)	0.59950 (13)	0.0208 (3)
O14	0.52129 (19)	−0.38231 (18)	0.79143 (16)	0.0293 (3)
O15	0.2915 (2)	0.0139 (2)	0.01415 (18)	0.0338 (4)
O16	0.5203 (3)	−0.0084 (3)	0.2382 (2)	0.0457 (5)
O17	0.4685 (3)	−0.3182 (3)	0.2952 (2)	0.0464 (5)
O18	−0.1556 (3)	0.6827 (2)	0.2455 (2)	0.0461 (5)
O19	0.4306 (3)	0.3289 (2)	−0.02683 (19)	0.0427 (5)
N1	0.3218 (3)	−0.7085 (3)	0.5108 (2)	0.0299 (4)
N2	−0.2163 (4)	0.3213 (3)	−0.0696 (2)	0.0407 (5)
H1	−0.116 (5)	0.592 (5)	0.284 (4)	0.064 (11)*
H2	−0.089 (5)	0.700 (5)	0.263 (4)	0.056 (12)*
H3	0.336 (5)	0.428 (5)	−0.078 (4)	0.062 (11)*
H4	−0.165 (5)	0.274 (4)	−0.110 (3)	0.045 (9)*
H5	0.413 (7)	0.290 (6)	0.039 (5)	0.094 (18)*
H6	0.438 (5)	0.030 (4)	0.269 (3)	0.038 (8)*
H7	0.378 (5)	−0.277 (4)	0.315 (3)	0.047 (10)*
H8	0.582 (6)	0.015 (5)	0.238 (4)	0.068 (14)*
H9	0.261 (9)	−0.752 (8)	0.552 (6)	0.14 (3)*
H10	0.497 (6)	−0.401 (5)	0.323 (4)	0.071 (14)*
H11	−0.310 (9)	0.298 (7)	−0.051 (6)	0.13 (2)*
H12	0.397 (6)	−0.748 (5)	0.485 (4)	0.063 (12)*
H13	0.235 (6)	0.031 (5)	0.070 (5)	0.077 (14)*
H14	−0.227 (8)	0.404 (7)	−0.106 (6)	0.11 (2)*
H15	0.270 (7)	−0.635 (7)	0.483 (5)	0.091 (18)*
H16	0.393 (10)	−0.692 (9)	0.559 (7)	0.16 (3)*
H17	0.229 (6)	0.018 (5)	−0.028 (5)	0.076 (15)*
H18	−0.159 (7)	0.293 (6)	−0.009 (5)	0.090 (17)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
V1	0.01847 (16)	0.01622 (15)	0.02018 (15)	−0.00716 (12)	0.00159 (11)	−0.00478 (11)
V2	0.01055 (14)	0.01234 (14)	0.01739 (15)	−0.00355 (11)	0.00123 (10)	−0.00643 (11)
V3	0.01947 (16)	0.01553 (15)	0.01686 (15)	−0.00556 (12)	0.00084 (11)	−0.00822 (11)
V4	0.01895 (16)	0.01236 (14)	0.02031 (16)	−0.00352 (11)	0.00098 (11)	−0.00810 (11)
V5	0.01465 (15)	0.01667 (15)	0.02257 (16)	−0.00286 (11)	−0.00286 (11)	−0.00488 (12)
Na	0.0331 (5)	0.0277 (4)	0.0359 (5)	−0.0124 (4)	0.0030 (4)	−0.0129 (4)
O1	0.0162 (6)	0.0183 (6)	0.0216 (6)	−0.0077 (5)	0.0028 (5)	−0.0070 (5)
O2	0.0139 (6)	0.0136 (5)	0.0180 (5)	−0.0046 (4)	0.0008 (4)	−0.0064 (4)
O3	0.0215 (6)	0.0190 (6)	0.0188 (6)	−0.0082 (5)	0.0041 (5)	−0.0084 (5)
O4	0.0218 (6)	0.0150 (6)	0.0228 (6)	−0.0074 (5)	0.0016 (5)	−0.0073 (5)
O5	0.0317 (8)	0.0260 (7)	0.0282 (7)	−0.0158 (6)	0.0062 (6)	−0.0057 (6)
O6	0.0203 (6)	0.0171 (6)	0.0219 (6)	−0.0056 (5)	−0.0015 (5)	−0.0045 (5)
O7	0.0135 (6)	0.0186 (6)	0.0242 (6)	−0.0042 (5)	0.0006 (5)	−0.0085 (5)
O8	0.0148 (5)	0.0144 (5)	0.0191 (6)	−0.0048 (4)	0.0004 (4)	−0.0080 (5)
O9	0.0147 (6)	0.0155 (6)	0.0194 (6)	−0.0044 (5)	0.0033 (4)	−0.0095 (5)
O10	0.0305 (7)	0.0269 (7)	0.0246 (7)	−0.0113 (6)	0.0047 (6)	−0.0165 (6)
O11	0.0182 (6)	0.0189 (6)	0.0205 (6)	−0.0054 (5)	−0.0024 (5)	−0.0077 (5)
O12	0.0290 (7)	0.0203 (7)	0.0315 (7)	−0.0064 (6)	0.0029 (6)	−0.0165 (6)
O13	0.0165 (6)	0.0154 (6)	0.0262 (6)	−0.0008 (5)	−0.0002 (5)	−0.0089 (5)
O14	0.0182 (6)	0.0253 (7)	0.0355 (8)	−0.0010 (6)	−0.0081 (6)	−0.0088 (6)
O15	0.0278 (8)	0.0423 (10)	0.0300 (8)	−0.0112 (7)	0.0039 (7)	−0.0153 (7)
O16	0.0365 (10)	0.0589 (13)	0.0742 (15)	−0.0281 (10)	0.0260 (10)	−0.0526 (12)
O17	0.0448 (11)	0.0332 (10)	0.0573 (13)	−0.0147 (9)	0.0267 (10)	−0.0164 (9)
O18	0.0410 (11)	0.0226 (8)	0.0674 (14)	−0.0096 (8)	−0.0162 (10)	−0.0100 (9)
O19	0.0513 (12)	0.0353 (10)	0.0308 (9)	−0.0049 (8)	−0.0034 (8)	−0.0132 (7)
N1	0.0264 (9)	0.0267 (9)	0.0403 (11)	−0.0083 (8)	0.0054 (8)	−0.0193 (8)
N2	0.0484 (14)	0.0296 (11)	0.0324 (11)	0.0003 (10)	−0.0031 (10)	−0.0152 (9)

Geometric parameters (Å, º) top

V1—O5	1.5963 (16)	Na—O16	2.338 (2)
V1—O6ⁱ	1.8516 (16)	Na—O19ⁱⁱ	2.340 (2)
V1—O4	1.8722 (15)	Na—O17	2.346 (2)
V1—O3	1.8887 (14)	Na—O18ⁱⁱⁱ	2.379 (3)
V1—O1	2.0181 (18)	Na—O15	2.404 (3)
V1—O2	2.3564 (15)	Na—O15ⁱⁱ	2.436 (2)
V1—V5ⁱ	3.0803 (9)	Na—Naⁱⁱ	3.394 (3)
V1—V2	3.0864 (17)	Na—H8	2.67 (4)
V2—O7	1.6862 (16)	O2—V2ⁱ	2.0971 (15)
V2—O1	1.7025 (15)	O2—V4ⁱ	2.2432 (13)
V2—O8	1.9184 (14)	O2—V5ⁱ	2.2917 (18)
V2—O9	1.9243 (14)	O4—V4ⁱ	1.8208 (15)
V2—O2ⁱ	2.0971 (15)	O6—V1ⁱ	1.8516 (16)
V2—O2	2.1147 (16)	O8—V4ⁱ	1.9939 (17)
V2—V5	3.0607 (16)	O8—V3ⁱ	2.0209 (15)
V3—O10	1.6223 (15)	O11—V3ⁱ	1.8178 (16)
V3—O3	1.8139 (15)	O15—Naⁱⁱ	2.436 (2)
V3—O11ⁱ	1.8178 (16)	O15—H13	0.80 (5)
V3—O9	1.9908 (17)	O15—H17	0.71 (5)
V3—O8ⁱ	2.0209 (15)	O16—H6	0.80 (4)
V3—O2	2.2301 (13)	O16—H8	0.66 (4)
V3—V4	3.0730 (17)	O17—H7	0.79 (4)
V3—V5ⁱ	3.1091 (13)	O17—H10	0.74 (5)
V4—O12	1.6158 (15)	O18—Na^iv	2.379 (3)
V4—O13	1.8199 (16)	O18—H1	0.82 (4)
V4—O4ⁱ	1.8208 (15)	O18—H2	0.71 (4)
V4—O8ⁱ	1.9939 (17)	O19—Naⁱⁱ	2.340 (2)
V4—O9	2.0010 (15)	O19—H3	1.01 (4)
V4—O2ⁱ	2.2432 (13)	O19—H5	0.74 (5)
V4—V5	3.0905 (10)	N1—H9	0.83 (7)
V5—O14	1.6039 (16)	N1—H12	0.73 (5)
V5—O6	1.8271 (16)	N1—H15	0.67 (6)
V5—O13	1.8677 (15)	N1—H16	0.93 (8)
V5—O11	1.8889 (15)	N2—H4	0.79 (4)
V5—O7	2.0521 (16)	N2—H11	0.92 (7)
V5—O2ⁱ	2.2917 (18)	N2—H14	0.78 (6)
V5—V1ⁱ	3.0803 (9)	N2—H18	0.75 (6)
V5—V3ⁱ	3.1091 (13)

O5—V1—O6ⁱ	104.49 (8)	O14—V5—O2ⁱ	172.35 (7)
O5—V1—O4	102.20 (8)	O6—V5—O2ⁱ	82.78 (6)
O6ⁱ—V1—O4	90.86 (7)	O13—V5—O2ⁱ	78.36 (6)
O5—V1—O3	103.63 (8)	O11—V5—O2ⁱ	77.43 (6)
O6ⁱ—V1—O3	89.89 (7)	O7—V5—O2ⁱ	74.50 (6)
O4—V1—O3	153.10 (6)	O14—V5—V2	129.13 (7)
O5—V1—O1	101.05 (8)	O6—V5—V2	126.01 (5)
O6ⁱ—V1—O1	154.46 (6)	O13—V5—V2	79.04 (5)
O4—V1—O1	83.92 (7)	O11—V5—V2	78.81 (5)
O3—V1—O1	83.90 (7)	O7—V5—V2	31.28 (4)
O5—V1—O2	174.98 (7)	O2ⁱ—V5—V2	43.23 (4)
O6ⁱ—V1—O2	80.48 (7)	O14—V5—V1ⁱ	138.24 (7)
O4—V1—O2	76.83 (5)	O6—V5—V1ⁱ	33.39 (5)
O3—V1—O2	76.79 (5)	O13—V5—V1ⁱ	84.98 (5)
O1—V1—O2	73.98 (6)	O11—V5—V1ⁱ	84.35 (5)
O5—V1—V5ⁱ	137.36 (7)	O7—V5—V1ⁱ	123.91 (5)
O6ⁱ—V1—V5ⁱ	32.89 (5)	O2ⁱ—V5—V1ⁱ	49.40 (4)
O4—V1—V5ⁱ	82.93 (5)	V2—V5—V1ⁱ	92.63 (4)
O3—V1—V5ⁱ	83.20 (5)	O14—V5—V4	133.32 (7)
O1—V1—V5ⁱ	121.58 (5)	O6—V5—V4	82.75 (5)
O2—V1—V5ⁱ	47.60 (4)	O13—V5—V4	32.58 (4)
O5—V1—V2	131.84 (6)	O11—V5—V4	123.81 (5)
O6ⁱ—V1—V2	123.67 (6)	O7—V5—V4	82.16 (5)
O4—V1—V2	78.43 (5)	O2ⁱ—V5—V4	46.38 (4)
O3—V1—V2	78.84 (5)	V2—V5—V4	61.85 (3)
O1—V1—V2	30.80 (4)	V1ⁱ—V5—V4	60.92 (2)
O2—V1—V2	43.18 (4)	O14—V5—V3ⁱ	134.60 (7)
V5ⁱ—V1—V2	90.78 (4)	O6—V5—V3ⁱ	81.71 (5)
O7—V2—O1	106.84 (8)	O13—V5—V3ⁱ	124.10 (5)
O7—V2—O8	97.30 (7)	O11—V5—V3ⁱ	32.28 (4)
O1—V2—O8	96.89 (7)	O7—V5—V3ⁱ	81.90 (5)
O7—V2—O9	97.21 (7)	O2ⁱ—V5—V3ⁱ	45.74 (4)
O1—V2—O9	96.84 (6)	V2—V5—V3ⁱ	61.77 (3)
O8—V2—O9	156.19 (6)	V1ⁱ—V5—V3ⁱ	60.62 (2)
O7—V2—O2ⁱ	87.64 (7)	V4—V5—V3ⁱ	91.86 (4)
O1—V2—O2ⁱ	165.51 (6)	O16—Na—O19ⁱⁱ	169.63 (9)
O8—V2—O2ⁱ	80.90 (6)	O16—Na—O17	88.05 (9)
O9—V2—O2ⁱ	80.94 (6)	O19ⁱⁱ—Na—O17	84.07 (9)
O7—V2—O2	166.09 (6)	O16—Na—O18ⁱⁱⁱ	88.84 (9)
O1—V2—O2	87.06 (7)	O19ⁱⁱ—Na—O18ⁱⁱⁱ	97.29 (9)
O8—V2—O2	80.80 (6)	O17—Na—O18ⁱⁱⁱ	85.95 (10)
O9—V2—O2	80.58 (6)	O16—Na—O15	83.16 (9)
O2ⁱ—V2—O2	78.45 (7)	O19ⁱⁱ—Na—O15	91.11 (8)
O7—V2—V5	39.19 (5)	O17—Na—O15	96.94 (9)
O1—V2—V5	146.03 (5)	O18ⁱⁱⁱ—Na—O15	171.37 (8)
O8—V2—V5	90.04 (5)	O16—Na—O15ⁱⁱ	84.40 (8)
O9—V2—V5	89.37 (4)	O19ⁱⁱ—Na—O15ⁱⁱ	104.39 (8)
O2ⁱ—V2—V5	48.46 (4)	O17—Na—O15ⁱⁱ	168.36 (9)
O2—V2—V5	126.90 (5)	O18ⁱⁱⁱ—Na—O15ⁱⁱ	85.05 (8)
O7—V2—V1	144.22 (5)	O15—Na—O15ⁱⁱ	90.95 (8)
O1—V2—V1	37.37 (5)	O16—Na—Naⁱⁱ	81.12 (8)
O8—V2—V1	89.40 (5)	O19ⁱⁱ—Na—Naⁱⁱ	101.08 (7)
O9—V2—V1	89.78 (4)	O17—Na—Naⁱⁱ	142.06 (8)
O2ⁱ—V2—V1	128.14 (4)	O18ⁱⁱⁱ—Na—Naⁱⁱ	129.67 (8)
O2—V2—V1	49.69 (5)	O15—Na—Naⁱⁱ	45.86 (6)
V5—V2—V1	176.591 (12)	O15ⁱⁱ—Na—Naⁱⁱ	45.09 (5)
O10—V3—O3	102.87 (7)	O16—Na—H8	13.0 (10)
O10—V3—O11ⁱ	102.47 (8)	O19ⁱⁱ—Na—H8	177.4 (10)
O3—V3—O11ⁱ	94.69 (7)	O17—Na—H8	97.6 (10)
O10—V3—O9	99.87 (7)	O18ⁱⁱⁱ—Na—H8	80.8 (10)
O3—V3—O9	91.10 (7)	O15—Na—H8	90.7 (10)
O11ⁱ—V3—O9	155.02 (6)	O15ⁱⁱ—Na—H8	73.7 (10)
O10—V3—O8ⁱ	99.48 (7)	Naⁱⁱ—Na—H8	78.9 (10)
O3—V3—O8ⁱ	155.82 (6)	V2—O1—V1	111.82 (8)
O11ⁱ—V3—O8ⁱ	89.35 (7)	V2ⁱ—O2—V2	101.55 (7)
O9—V3—O8ⁱ	76.00 (6)	V2ⁱ—O2—V3	94.05 (5)
O10—V3—O2	174.29 (7)	V2—O2—V3	92.95 (5)
O3—V3—O2	81.63 (6)	V2ⁱ—O2—V4ⁱ	93.44 (5)
O11ⁱ—V3—O2	80.47 (6)	V2—O2—V4ⁱ	92.84 (5)
O9—V3—O2	76.36 (6)	V3—O2—V4ⁱ	169.44 (7)
O8ⁱ—V3—O2	75.54 (5)	V2ⁱ—O2—V5ⁱ	88.32 (6)
O10—V3—V4	89.63 (6)	V2—O2—V5ⁱ	170.12 (7)
O3—V3—V4	130.88 (5)	V3—O2—V5ⁱ	86.87 (5)
O11ⁱ—V3—V4	129.08 (6)	V4ⁱ—O2—V5ⁱ	85.91 (5)
O9—V3—V4	39.78 (5)	V2ⁱ—O2—V1	171.31 (6)
O8ⁱ—V3—V4	39.73 (4)	V2—O2—V1	87.13 (6)
O2—V3—V4	84.74 (4)	V3—O2—V1	85.81 (5)
O10—V3—V5ⁱ	136.02 (6)	V4ⁱ—O2—V1	85.67 (5)
O3—V3—V5ⁱ	83.49 (5)	V5ⁱ—O2—V1	83.00 (6)
O11ⁱ—V3—V5ⁱ	33.71 (5)	V3—O3—V1	115.04 (7)
O9—V3—V5ⁱ	123.72 (5)	V4ⁱ—O4—V1	115.78 (7)
O8ⁱ—V3—V5ⁱ	86.83 (5)	V5—O6—V1ⁱ	113.72 (8)
O2—V3—V5ⁱ	47.39 (4)	V2—O7—V5	109.53 (8)
V4—V3—V5ⁱ	119.13 (3)	V2—O8—V4ⁱ	107.64 (7)
O12—V4—O13	103.01 (8)	V2—O8—V3ⁱ	106.99 (6)
O12—V4—O4ⁱ	103.52 (7)	V4ⁱ—O8—V3ⁱ	99.89 (7)
O13—V4—O4ⁱ	95.11 (7)	V2—O9—V3	107.19 (7)
O12—V4—O8ⁱ	99.52 (7)	V2—O9—V4	107.28 (6)
O13—V4—O8ⁱ	155.07 (6)	V3—O9—V4	100.68 (7)
O4ⁱ—V4—O8ⁱ	89.83 (7)	V3ⁱ—O11—V5	114.01 (7)
O12—V4—O9	99.23 (7)	V4—O13—V5	113.87 (7)
O13—V4—O9	89.53 (7)	Na—O15—Naⁱⁱ	89.05 (8)
O4ⁱ—V4—O9	155.08 (6)	Na—O15—H13	104 (3)
O8ⁱ—V4—O9	76.38 (6)	Naⁱⁱ—O15—H13	126 (3)
O12—V4—O2ⁱ	173.92 (7)	Na—O15—H17	137 (4)
O13—V4—O2ⁱ	80.62 (6)	Naⁱⁱ—O15—H17	104 (4)
O4ⁱ—V4—O2ⁱ	80.84 (6)	H13—O15—H17	101 (5)
O8ⁱ—V4—O2ⁱ	76.07 (6)	Na—O16—H6	131 (2)
O9—V4—O2ⁱ	75.77 (5)	Na—O16—H8	114 (4)
O12—V4—V3	89.19 (6)	H6—O16—H8	114 (5)
O13—V4—V3	129.06 (6)	Na—O17—H7	116 (3)
O4ⁱ—V4—V3	130.21 (5)	Na—O17—H10	130 (3)
O8ⁱ—V4—V3	40.38 (5)	H7—O17—H10	112 (4)
O9—V4—V3	39.54 (4)	Na^iv—O18—H1	126 (3)
O2ⁱ—V4—V3	84.75 (4)	Na^iv—O18—H2	133 (3)
O12—V4—V5	136.39 (6)	H1—O18—H2	101 (4)
O13—V4—V5	33.55 (5)	Naⁱⁱ—O19—H3	105 (2)
O4ⁱ—V4—V5	83.41 (5)	Naⁱⁱ—O19—H5	101 (4)
O8ⁱ—V4—V5	123.76 (5)	H3—O19—H5	115 (4)
O9—V4—V5	87.15 (5)	H9—N1—H12	121 (5)
O2ⁱ—V4—V5	47.70 (4)	H9—N1—H15	107 (6)
V3—V4—V5	119.30 (3)	H12—N1—H15	125 (5)
O14—V5—O6	104.86 (8)	H9—N1—H16	116 (6)
O14—V5—O13	100.76 (8)	H12—N1—H16	89 (5)
O6—V5—O13	92.52 (7)	H15—N1—H16	94 (6)
O14—V5—O11	102.34 (8)	H4—N2—H11	105 (4)
O6—V5—O11	90.98 (7)	H4—N2—H14	108 (5)
O13—V5—O11	154.88 (6)	H11—N2—H14	121 (6)
O14—V5—O7	97.85 (8)	H4—N2—H18	107 (5)
O6—V5—O7	157.28 (6)	H11—N2—H18	110 (5)
O13—V5—O7	83.77 (6)	H14—N2—H18	106 (5)
O11—V5—O7	83.46 (6)

Symmetry codes: (i) −x, −y, −z+1; (ii) −x+1, −y, −z; (iii) x+1, y−1, z; (iv) x−1, y+1, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H12···O7^v	0.73 (5)	2.14 (5)	2.862 (3)	175 (4)
N1—H15···O12	0.67 (6)	2.26 (6)	2.910 (3)	164 (6)
N1—H9···O8^vi	0.83 (7)	2.17 (7)	2.944 (3)	156 (6)
N2—H14···O14^vii	0.77 (6)	2.35 (6)	2.899 (3)	129 (5)
N2—H4···O10^viii	0.79 (4)	2.17 (4)	2.933 (3)	165 (3)
N2—H11···O19^ix	0.92 (7)	2.12 (7)	2.993 (4)	159 (6)
O15—H17···O10^viii	0.71 (5)	2.35 (5)	3.039 (3)	165 (5)
O15—H13···O3	0.80 (5)	2.08 (5)	2.855 (2)	163 (5)
O16—H8···O11^x	0.66 (4)	2.18 (4)	2.833 (3)	168 (5)
O16—H6···O1	0.80 (3)	2.06 (4)	2.860 (3)	174 (3)
O17—H10···O13^v	0.74 (5)	2.17 (5)	2.867 (3)	159 (5)
O17—H7···O9	0.79 (4)	2.21 (4)	2.952 (3)	157 (4)
O18—H2···O10^xi	0.71 (4)	2.42 (4)	2.974 (3)	136 (4)
O18—H1···O4	0.82 (4)	1.99 (4)	2.801 (3)	176 (4)
O19—H5···O14^x	0.74 (5)	2.61 (5)	2.982 (3)	113 (5)
O19—H3···O6^xii	1.01 (4)	1.80 (4)	2.795 (3)	168 (3)

Symmetry codes: (v) −x+1, −y−1, −z+1; (vi) x, y−1, z; (vii) x−1, y+1, z−1; (viii) −x, −y, −z; (ix) x−1, y, z; (x) −x+1, −y, −z+1; (xi) x, y+1, z; (xii) x, y+1, z−1.

Experimental details

Crystal data
Chemical formula	(NH₄)₄[Na₂(H₂O)₁₀][V₁₀O₂₈]
M_r	1255.71
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	8.501 (2), 10.426 (2), 11.282 (2)
α, β, γ (°)	68.46 (3), 87.30 (3), 67.14 (3)
V (Å³)	851.7 (3)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	2.77
Crystal size (mm)	0.2 × 0.2 × 0.1

Data collection
Diffractometer	Enraf-Nonius CAD-4 diffractometer
Absorption correction	ψ scan (CORINC; Schollmeyer, 1992)
T_min, T_max	0.632, 0.758
No. of measured, independent and observed [I > 2σ(I)] reflections	5282, 4933, 4474
R_int	0.007
(sin θ/λ)_max (Å⁻¹)	0.703

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.036, 0.102, 1.06
No. of reflections	4933
No. of parameters	316
H-atom treatment	All H-atom parameters refined
Δρ_max, Δρ_min (e Å⁻³)	1.31, −1.17

Computer programs: CAD-4 Software (Enraf-Nonius, 1989), CAD-4 Software, CORINC (Schollmeyer, 1992), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), DIAMOND (Bergerhoff, 1996), SHELXL97.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H12···O7ⁱ	0.73 (5)	2.14 (5)	2.862 (3)	175 (4)
N1—H15···O12	0.67 (6)	2.26 (6)	2.910 (3)	164 (6)
N1—H9···O8ⁱⁱ	0.83 (7)	2.17 (7)	2.944 (3)	156 (6)
N2—H14···O14ⁱⁱⁱ	0.77 (6)	2.35 (6)	2.899 (3)	129 (5)
N2—H4···O10^iv	0.79 (4)	2.17 (4)	2.933 (3)	165 (3)
N2—H11···O19^v	0.92 (7)	2.12 (7)	2.993 (4)	159 (6)
O15—H17···O10^iv	0.71 (5)	2.35 (5)	3.039 (3)	165 (5)
O15—H13···O3	0.80 (5)	2.08 (5)	2.855 (2)	163 (5)
O16—H8···O11^vi	0.66 (4)	2.18 (4)	2.833 (3)	168 (5)
O16—H6···O1	0.80 (3)	2.06 (4)	2.860 (3)	174 (3)
O17—H10···O13ⁱ	0.74 (5)	2.17 (5)	2.867 (3)	159 (5)
O17—H7···O9	0.79 (4)	2.21 (4)	2.952 (3)	157 (4)
O18—H2···O10^vii	0.71 (4)	2.42 (4)	2.974 (3)	136 (4)
O18—H1···O4	0.82 (4)	1.99 (4)	2.801 (3)	176 (4)
O19—H5···O14^vi	0.74 (5)	2.61 (5)	2.982 (3)	113 (5)
O19—H3···O6^viii	1.01 (4)	1.80 (4)	2.795 (3)	168 (3)

Symmetry codes: (i) −x+1, −y−1, −z+1; (ii) x, y−1, z; (iii) x−1, y+1, z−1; (iv) −x, −y, −z; (v) x−1, y, z; (vi) −x+1, −y, −z+1; (vii) x, y+1, z; (viii) x, y+1, z−1.

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