Redetermination of diammonium thio­molybdate

Hill, B.; Lerner, H.-W.; Bolte, M.

doi:10.1107/S1600536810003016

Volume 66
Part 2
Page i13
February 2010

Received 6 January 2010
Accepted 25 January 2010
Online 30 January 2010

Key indicators
Single-crystal X-ray study
T = 173 K
Mean (Mo-S) = 0.001 Å
R = 0.022
wR = 0.060
Data-to-parameter ratio = 14.1
Details

Redetermination of diammonium thiomolybdate

Björn Hill,^a Hans-Wolfram Lerner ^a and Michael Bolte ^a ^*

^aInstitut für Anorganische Chemie der Goethe-Universität Frankfurt, Max-von-Laue-Strasse 7, D-60438 Frankfurt am Main, Germany
Correspondence e-mail: bolte@chemie.uni-frankfurt.de

In contrast to the previous structure determinations of the title structure, (NH₄)₂[MoS₄], the present determination at 173 K localized the positions of the H atoms. The title structure belongs to the [beta] -K₂SO₄ family and all the ions are located on crystallographic mirror planes. The ions are held together by N-HS hydrogen bonds (some of which are bifurcated), forming a three-dimensional network. One of the N atoms has nine contacts to the S atoms shorter than 4 Å, and the other has ten.

Related literature

For preparation of the title compound, see: Herzog et al. (1981). For structures of the [beta] -K₂SO₄ family, see: Fábry & Pérez-Mato (1994). For other structure determinations of the title compound, see: Lapasset et al. (1976); Schäfer et al. (1964). For a description of the Cambridge Structural Database, see: Allen (2002).

Experimental

Crystal data

(NH₄)₂[MoS₄]
M_r = 260.26
Orthorhombic, P n m a
a = 9.5867 (4) Å
b = 6.9451 (4) Å
c = 12.2005 (5) Å
V = 812.32 (7) Å³
Z = 4
Mo K radiation
= 2.55 mm^-1
T = 173 K
0.25 × 0.24 × 0.11 mm

Data collection

Stoe IPDS II two-circle diffractometer
Absorption correction: multi-scan (MULABS; Spek, 2009; Blessing, 1995) T_min = 0.569, T_max = 0.767
14872 measured reflections
859 independent reflections
833 reflections with I > 2(I)
R_int = 0.072

Refinement

R[F² > 2(F²)] = 0.022
wR(F²) = 0.060
S = 1.19
859 reflections
61 parameters
6 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 0.51 e Å^-3
_min = -0.88 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N1-H1AS1ⁱ	0.86 (2)	2.76 (4)	3.491 (3)	144 (6)
N1-H1BS1ⁱⁱ	0.88 (2)	2.92 (5)	3.607 (3)	135 (5)
N1-H1BS3	0.88 (2)	2.87 (3)	3.497 (3)	129 (3)
N1-H1BS3ⁱⁱⁱ	0.88 (2)	2.87 (3)	3.497 (3)	129 (3)
N1-H1CS3^iv	0.88 (2)	2.76 (3)	3.550 (3)	150 (4)
N1-H1CS3^iv	0.88 (2)	2.76 (3)	3.550 (3)	150 (4)
N2-H2CS3^v	0.88 (2)	2.65 (3)	3.405 (2)	144 (4)
N2-H2AS3^vi	0.88 (2)	2.76 (2)	3.481 (2)	140 (1)
N2-H2AS3^vii	0.88 (2)	2.76 (2)	3.481 (2)	140 (1)
N2-H2BS1	0.88 (2)	2.61 (4)	3.414 (3)	153 (6)
N2-H2BS2	0.88 (2)	2.70 (6)	3.250 (3)	122 (5)
Symmetry codes: (i) x+1, y, z; (ii) $[x+{\script{1\over 2}}, y, -z+{\script{1\over 2}}]$ ; (iii) $[x, -y+{\script{3\over 2}}, z]$ ; (iv) $[-x+1, y+{\script{1\over 2}}, -z+1]$ ; (v) -x, -y+1, -z+1; (vi) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (vii) $[-x+{\script{1\over 2}}, -y+1, z+{\script{1\over 2}}]$ .

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2009).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: FB2179 ).

References

Allen, F. H. (2002). Acta Cryst. B58, 380-388.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Fábry, J. & Pérez-Mato, J. M. (1994). Phase Trans. 499, 193-229.
Herzog, S., Gustav, K. & Strähle, J. (1981). Handbuch der Präparativen Chemie, Vol. 3, edited by G. Brauer, pp. 1551-1552. Stuttgart: Ferdinand Enke Verlag.
Lapasset, J., Chezau, N. & Belougne, P. (1976). Acta Cryst. B32, 3087-3088.
Schäfer, H., Schäfer, G. & Weiss, A. (1964). Z. Naturforsch. Teil B, 19, 76.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148-155.
Stoe & Cie (2001). X-AREA and X-RED. Stoe & Cie, Darmstadt, Germany.

inorganic compounds