(IUCr) The solid solution Na0.39(NH4)1.61SO4·Te(OH)6

Volume 64
Part 3
Pages i18-i19
March 2008

Received 14 December 2007
Accepted 31 January 2008
Online 6 February 2008

Key indicators
Single-crystal X-ray study
T = 298 K
Mean (S-O) = 0.005 Å
H completeness 60%
Disorder in main residue
R = 0.032
wR = 0.044
Data-to-parameter ratio = 6.1
Details

The solid solution Na_0.39(NH₄)_1.61SO₄·Te(OH)₆

Lilia Ktari,^a Mohamed Abdelhedi,^a,^b ^* Mohamed Dammak,^a Alain Cousson ^b and Abdelwaheb Kolsi ^a

^aLaboratoire de Chimie Inorganique, Faculté des Sciences de Sfax, 3018 Sfax, Tunisia, and ^bLaboratoire Léon Brillouin, CE Saclay, Bâtiment 563, 91191 Gif-sur-Yvette Cedex, France
Correspondence e-mail: m_abdelhedi2002@yahoo.fr

The title compound, sodium ammonium sulfate-telluric acid (1/1), Na_0.39(NH₄)_1.61SO₄·Te(OH)₆, is isostructural with other solid solutions in the series M_1-x(NH₄)_xSO₄·Te(OH)₆, where ammonium is partially replaced with an alkali metal (M = K, Rb or Cs). The structure is composed of planes of Te(OH)₆ octahedra alternating with planes of SO₄ tetrahedra. The Na⁺/NH₄⁺ cations are statistically distributed over the same position and are located between the planes. The structure is stabilized by O-HO and N-HO hydrogen bonds between the telluric acid adducts and the O atoms of sulfate groups, and between the ammonium cations and O atoms, respectively. Both Te atoms lie on centres of symmetry.

Related literature

For the sodium end-member of the solid solution series Na_1-x(NH₄)_xSO₄·Te(OH)₆, see: Zilber et al. (1980). For the ammonium end-member of the same series, see: Zilber et al. (1981). For other solid solutions in the system M_1-x(NH₄)_xSO₄·Te(OH)₆, where ammonium is partially replaced by an alkali metal, see: Dammak et al. (2005) for M = Cs; Ktari et al. (2002) for M = Rb; and Ktari et al. (2004) for M = K. For related literature, see: Prince (1982); Watkin (1994).

Experimental

Crystal data

Na_0.39(NH₄)_1.61SO₄·Te(OH)₆
M_r = 357.22
Monoclinic, P 2₁ /c
a = 13.690 (1) Å
b = 6.592 (1) Å
c = 11.345 (1) Å
= 106.58 (1)°
V = 981.26 (19) Å³
Z = 4
Mo K radiation
= 3.30 mm^-1
T = 298 K
0.15 × 0.14 × 0.10 mm

Data collection

Nonius KappaCCD diffractometer
Absorption correction: multi-scan (MULABS in PLATON; Spek, 2007) T_min = 0.615, T_max = 0.719
919 measured reflections
849 independent reflections
638 reflections with I > 3(I)
R_int = 0.000

Refinement

R[F² > 2(F²)] = 0.032
wR(F²) = 0.043
S = 0.93
638 reflections
104 parameters
1 restraint
H-atom parameters constrained
_max = 0.51 e Å^-3
_min = -1.15 e Å^-3

Table 1
Selected bond lengths (Å)

Te1-O1	1.903 (6)
Te1-O2	1.905 (4)
Te1-O3	1.916 (3)
Te2-O4	1.914 (3)
Te2-O5	1.915 (4)
Te2-O6	1.904 (5)
S1-O7	1.486 (6)
S1-O8	1.485 (3)
S1-O9	1.474 (3)
S1-O10	1.460 (6)
Na1-O6ⁱ	2.873 (4)
Na1-O4ⁱⁱ	2.937 (6)
Na1-O5ⁱⁱⁱ	2.947 (4)
Na1-O3^iv	2.950 (4)
Na1-O7^v	2.978 (7)
Na1-O10^vi	3.008 (4)
Na1-O9	3.120 (4)
Na1-O6ⁱⁱ	3.267 (6)
Na1-O5^vii	3.278 (5)
Na2-O9	2.938 (5)
Na2-O8^vi	2.966 (4)
Na2-O4ⁱⁱ	3.029 (4)
Na2-O10^viii	3.037 (7)
Na2-O2^ix	3.050 (4)
Na2-O2^x	3.063 (5)
Na2-O1^xi	3.144 (5)
Na2-O3^vii	3.164 (5)
Na2-O1^iv	3.305 (6)
Symmetry codes: (i) $[-x, y-{\script{3\over 2}}, -z-{\script{1\over 2}}]$ ; (ii) x, y-1, z; (iii) $[x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (iv) $[-x, y-{\script{1\over 2}}, -z-{\script{1\over 2}}]$ ; (v) $[x, -y-{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (vi) x, y+1, z; (vii) -x, -y+1, -z; (viii) $[x, -y-{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (ix) x-1, y, z; (x) -x, -y, -z; (xi) x-1, y-1, z.

Table 2
Hydrogen-bond and short contact geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O2-H2O9^xii	0.924 (4)	1.787 (4)	2.700 (6)	169.2 (2)
O3-H3O8^xiii	0.985 (5)	1.871 (5)	2.799 (7)	155.7 (2)
O4-H4O7^xiv	0.937 (3)	1.798 (3)	2.706 (7)	162.4 (2)
O6-H6O10^xiii	0.963 (4)	1.706 (4)	2.658 (6)	169.5 (3)
N1.O6ⁱ			2.873 (4)
N1O4ⁱⁱ			2.937 (6)
N1O5ⁱⁱⁱ			2.947 (4)
N1O3^iv			2.950 (4)
N1O7^v			2.978 (7)
N1O10^vi			3.008 (4)
N2O9			2.938 (5)
N2O8^vi			2.966 (4)
N2O4ⁱⁱ			3.029 (4)
N2O10^viii			3.037 (7)
N2O2^ix			3.050 (4)
N2O2^x			3.063 (5)
Symmetry codes: (i) $[-x, y-{\script{3\over 2}}, -z-{\script{1\over 2}}]$ ; (ii) x, y-1, z; (iii) $[x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (iv) $[-x, y-{\script{1\over 2}}, -z-{\script{1\over 2}}]$ ; (v) $[x, -y-{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (vi) x, y+1, z; (viii) $[x, -y-{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (ix) x-1, y, z; (x) -x, -y, -z; (xii) $[-x, y+{\script{1\over 2}}, -z-{\script{1\over 2}}]$ ; (xiii) $[-x, y+{\script{3\over 2}}, -z-{\script{1\over 2}}]$ ; (xiv) x, y+2, z.

Data collection: COLLECT (Nonius, 2001); cell refinement: DENZO/SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO/SCALEPACK; program(s) used to solve structure: SHELXS86 (Sheldrick, 2008); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: DIAMOND (Brandenburg & Berndt, 1999); software used to prepare material for publication: CRYSTALS.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2171 ).

Acknowledgements

This project was supported by the French Ministry of Research and New Technologies and the French/Tunisian Twin Committee for University Collaboration.

References

Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487.
Brandenburg, K. & Berndt, M. (1999). DIAMOND. Version 2.1b. Crystal Impact GbR, Bonn, Germany.
Dammak, M., Ktari, L., Cousson, A. & Mhiri, T. (2005). J. Solid State Chem. 178, 2109-2116.
Ktari, L., Dammak, M., Hadrich, A., Cousson, A., Nierlich, M., Romain, F. & Mhiri, T. (2004). Solid State Sci. 6, 1393-1401.
Ktari, L., Dammak, M., Mhiri, T. & Kolsi, A. W. (2002). Phys. Chem. News, 8, 1-8.
Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.
Prince, E. (1982). Mathematical Techniques in Crystallography and Materials Science. New York: Springer-Verlag.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2007). PLATON. Utrecht University, The Netherlands.
Watkin, D. (1994). Acta Cryst. A50, 411-437.
Zilber, R., Durif, A. & Averbuch-Pouchot, M. T. (1981). Acta Cryst. B37, 650-652.
Zilber, R., Tordjman, I. & Guitel, J. C. (1980). Acta Cryst. B36, 2741-2743.

inorganic compounds

The solid solution Na0.39(NH4)1.61SO4·Te(OH)6