Bis[benzyl(methyl)ammonium] tetrathiomolybdate(VI)

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Acta Crystallographica Section E

Structure Reports Online

ISSN 1600-5368

Editors:W. Clegg and D. G. Watson

Bis[benzyl(methyl)ammonium] tetrathiomolybdate(VI)

Bikshandarkoil R. Srinivasan, Siddhali V. Girkar and Pallepogu Raghavaiah

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Acta Cryst.(2007). E63, m2737–m2738 Srinivasanet al. ^¯ (C₈H₁₂N)₂[MoS₄]

Bis[benzyl(methyl)ammonium] tetrathio- molybdate(VI)

Bikshandarkoil R. Srinivasan,* Siddhali V. Girkar and Pallepogu Raghavaiah

Department of Chemistry, Goa University, Goa 403 206, India Correspondence e-mail: srini@unigoa.ac.in

Received 7 October 2007; accepted 9 October 2007

Key indicators: single-crystal X-ray study;T= 298 K; mean(C–C) = 0.009 A˚;

Rfactor = 0.050;wRfactor = 0.100; data-to-parameter ratio = 17.3.

The title compound, (C8H12N)2[MoS4], was synthesized by the aqueous reaction of ammonium tetrathiomolybdate with benzyl(methyl)amine in a 1:2 molar ratio. The structure consists of a slightly distorted tetrahedral [MoS4]² dianion and two crystallographically independent benzyl(methyl)- ammonium cations, with all atoms located in general positions.

The cations and anions are linked by weak N—H S and C—

H S interactions, the strength and number of which can explain the observed Mo—S bond distances.

Related literature

Previous reports give details of the structural characterization of several organic ammonium tetrathiomolybdates derived from organic diamines (Srinivasan et al., 2001; Srinivasan, Dhuriet al., 2005; Srinivasan, Na¨ther & Bensch, 2005), chiral amines (Srinivasan, Naik et al., 2007), triamines (Srinivasan, Dhuri et al., 2007), cyclic amines (Srinivasan, Na¨ther &

Bensch, 2006), a tetraamine (Srinivasan et al., 2004) and a primary amine (Srinivasan, Na¨theret al., 2006).

Experimental Crystal data (C8H12N)2[MoS4] M_r= 468.55 Triclinic,P1 a= 7.1857 (12) A˚ b= 10.7376 (18) A˚ c= 14.881 (2) A˚ = 110.811 (2) = 90.608 (3)

= 100.504 (3) V= 1051.7 (3) A˚³ Z= 2

MoKradiation = 1.02 mm¹ T= 298 (2) K 0.420.060.02 mm

Data collection

Bruker SMART APEX CCD diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 2004) T_min= 0.901,T_max= 0.976

7363 measured reflections 3639 independent reflections 3015 reflections withI> 2(I) R_int= 0.035

Refinement

R[F²> 2(F²)] = 0.050 wR(F²) = 0.100 S= 1.05 3639 reflections

210 parameters

H-atom parameters constrained max= 0.68 e A˚³

min=0.51 e A˚³

Table 1

Selected geometric parameters (A˚ ,).

Mo1—S1 2.1582 (13)

Mo1—S2 2.1597 (16)

Mo1—S3 2.1888 (14)

Mo1—S4 2.1908 (14)

S1—Mo1—S2 109.43 (6)

S1—Mo1—S3 109.32 (6)

S2—Mo1—S3 110.28 (7)

S1—Mo1—S4 109.47 (5)

S2—Mo1—S4 109.01 (6)

S3—Mo1—S4 109.31 (6)

Table 2

Hydrogen-bond geometry (A˚ ,).

D—H A D—H H A D A D—H A

N1—H1A S3ⁱ 0.90 2.51 3.308 (4) 149

N1—H1A S1ⁱ 0.90 2.78 3.358 (4) 124

N1—H1B S4 0.90 2.37 3.253 (4) 168

N2—H2A S4 0.90 2.48 3.305 (5) 153

N2—H2B S4ⁱⁱ 0.90 2.54 3.264 (5) 138

N2—H2B S2ⁱⁱ 0.90 2.93 3.602 (5) 132

C7—H7B S3 0.97 2.92 3.727 (6) 141

C15—H15A S1ⁱⁱⁱ 0.97 2.91 3.629 (6) 132

Symmetry codes: (i)xþ1;y;z; (ii)xþ1;yþ1;zþ1; (iii)x;yþ1;zþ1.

Data collection:SMART(Bruker, 2001); cell refinement:SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Branden- burg 1999); software used to prepare material for publication:

SHELXTL.

This work was supported by the Department of Science and Technology (DST), New Delhi, under grant No. SR/S1/IC-41/

2003. BRS thanks Dr Samar K. Das, School of Chemistry, University of Hyderabad, for the X-ray intensity data collec- tion.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NC2064).

References

Brandenburg, K. (1999). DIAMOND. Release 2.1c. Crystal Impact GbR, Bonn, Germany.

Bruker (2001).SMARTandSAINT. Bruker AXS Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (2001).SHELXTL. Version 5.0. Bruker AXS Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (2004).SADABS. University of Go¨ttingen, Germany.

metal-organic compounds

Acta Crystallographica Section E

Structure Reports Online

ISSN 1600-5368

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Polyhedron,26doi:10.1016//j.poly.2007.08.023.

Srinivasan, B. R., Dhuri, S. N., Na¨ther, C. & Bensch, W. (2005).Inorg. Chim.

Acta,358, 279–287.

Srinivasan, B. R., Dhuri, S. N., Poisot, M., Na¨ther, C. & Bensch, W. (2004).Z.

Naturforsch. Teil B,59, 1083–1092.

Srinivasan, B. R., Naik, A. R., Na¨ther, C. & Bensch, W. (2007).Z. Anorg. Allg.

Chem.633, 582–588.

Srinivasan, B. R., Na¨ther, C., Naik, A. R. & Bensch, W. (2006).Acta Cryst.E62, m1635–m1637.

Srinivasan, B. R., Na¨ther, C. & Bensch, W. (2005).Acta Cryst.E61, m2454–

m2456.

Srinivasan, B. R., Na¨ther, C. & Bensch, W. (2006). Acta Cryst.C62, m98–

m101.

Srinivasan, B. R., Vernekar, B. K. & Nagarajan, K. (2001).Indian J. Chem.

Sect. A,40, 563–567.

metal-organic compounds

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