Triclinic modification of tetra­kis­(triethyl­ammonium) dihydrogeno­deca­vanadate(V)

Ng, S.W.

doi:10.1107/S1600536811019696

Volume 67
Part 6
Pages m811-m812
June 2011

Received 12 May 2011
Accepted 24 May 2011
Online 28 May 2011

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.007 Å
Disorder in solvent or counterion
R = 0.049
wR = 0.133
Data-to-parameter ratio = 16.6
Details

Triclinic modification of tetrakis(triethylammonium) dihydrogenodecavanadate(V)

Seik Weng Ng ^a ^*

^aDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
Correspondence e-mail: seikweng@um.edu.my

In the title ammonium polyoxometallate salt, (C₆H₁₆N)₄[H₂V₁₀O₂₈], the anion features O atoms engaged in [mu] ₆-, [mu] ₃- and [mu] ₂-bridging of adjacent V^V atoms, confering an octahedral coordination at each of the twenty unique metal atoms. Two anions are linked by [mu] ₃- and [mu] ₂-bridged OH units across a center of inversion, forming a dimer which is linked to the cations by N-HO hydrogen bonds. The cation is disordered over two positions in a 0.776 (4):0.224 (4) ratio in one of the two independent ion pairs in the asymmetric unit, and 0.627 (10):0.373 (10) in the other.

Related literature

For the monoclinic modification, see: Correia et al. (2004); Sarkar & Pal (2008).

Experimental

Crystal data

(C₆H₁₆N)₄[H₂V₁₀O₂₈]
M_r = 1368.21
Triclinic, $[P \overline 1]$
a = 13.1735 (4) Å
b = 20.0061 (7) Å
c = 20.2427 (7) Å
= 62.669 (3)°
= 86.263 (3)°
= 76.979 (3)°
V = 4613.0 (3) Å³
Z = 4
Mo K radiation
= 2.02 mm^-1
T = 100 K
0.20 × 0.15 × 0.10 mm

Data collection

Agilent SuperNova Dual diffractometer with an Atlas detector
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2010) T_min = 0.688, T_max = 0.824
38533 measured reflections
20465 independent reflections
13087 reflections with I > 2(I)
R_int = 0.041

Refinement

R[F² > 2(F²)] = 0.049
wR(F²) = 0.133
S = 1.04
20465 reflections
1230 parameters
132 restraints
H-atom parameters constrained
_max = 1.47 e Å^-3
_min = -0.79 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N1-H1O3	0.88	2.06	2.937 (4)	175
N2-H2O14	0.88	1.89	2.765 (4)	176
N3-H3O41	0.88	1.82	2.699 (4)	175
N4-H4O9	0.88	2.13	2.968 (9)	160
N4'-H4'O9	0.88	1.99	2.830 (16)	158
N5-H5O26	0.88	2.39	2.981 (5)	125
N5-H5O28	0.88	2.38	3.187 (5)	153
N6-H6O51	0.88	1.96	2.823 (4)	167
N7-H7O34	0.88	2.33	3.061 (4)	141
N7-H7O45	0.88	2.44	3.156 (5)	139
N7-H7O46	0.88	2.40	3.139 (4)	142
N8-H8O52	0.88	1.91	2.766 (4)	162
O15-H15O18ⁱ	0.84	1.99	2.819 (4)	171
O17-H17O16ⁱ	0.84	1.90	2.715 (4)	162
O54-H54O55ⁱⁱ	0.84	1.88	2.686 (4)	159
O56-H56O53ⁱⁱ	0.84	1.94	2.775 (4)	177
Symmetry codes: (i) -x+1, -y+1, -z; (ii) -x+2, -y, -z+2.

Data collection: CrysAlis PRO (Agilent, 2010); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: ZS2113 ).

Acknowledgements

I thank the University of Malaya for supporting this study.

References

Agilent (2010). CrysAlis PRO. Agilent Technologies, Yarnton, England.
Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.
Correia, I., Avecilla, F., Marcão, S. & Pessoa, J. C. (2004). Inorg. Chim. Acta, 357, 4476-4487.
Sarkar, A. & Pal, S. (2008). Polyhedron, 27, 3472-3476.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.

metal-organic compounds