electronic reprint
Acta Crystallographica Section E
Structure Reports Online
ISSN 1600-5368
Editors:W. Clegg and D. G. Watson
Cs
2[WS
4]
Bikshandarkoil R. Srinivasan, Christian N¨ather and Wolfgang Bensch
Copyright © International Union of Crystallography
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Acta Cryst.(2007). E63, i167 Srinivasanet al. ¯ Cs2[WS4]
Cs
2[WS
4]
Bikshandarkoil R. Srinivasan,a* Christian Na¨therband Wolfgang Benschb
aDepartment of Chemistry, Goa University PO, Goa 403 206, India, andbInstitut fu¨r Anorganische Chemie, Christian-Albrechts-Universita¨t Kiel, Olshausenstrasse 40, D-24098 Kiel, Germany
Correspondence e-mail: srini@unigoa.ac.in Received 19 June 2007; accepted 25 June 2007
Key indicators: single-crystal X-ray study;T= 170 K; mean(W–S) = 0.002 A˚;
Rfactor = 0.027;wRfactor = 0.069; data-to-parameter ratio = 36.4.
The title compound, dicaesium tetrathiotungstate(VI), was obtained from a dilute aqueous solution containing equimolar quantities of Cs2CO3 and (NH4)2[WS4]. The compound crystallizes in the orthorhombic space group Pnma and is isotypic with Cs2[MoS4], Rb2[WS4], (NH4)2[WS4] and K2[MoS4]. The structure contains discrete slightly distorted tetrahedral [WS4]2 anions (msymmetry), separated by Cs+ cations. One of the two unique Cs+cations (both located on mirror planes) is surrounded by nine S atoms and the other by ten S atoms.
Related literature
The title compound has previously been characterized by X-ray powder diffraction (Mu¨ller & Sievert, 1974). For isotypic structures see: Cs2[MoS4] (Raymond et al., 1995), K2[MoS4] (Emirdag-Eanes & Ibers, 2001), Rb2[MoS4] (Eller- meier et al., 1999), Rb2[WS4] (Yao & Ibers, 2004) and (NH4)2[WS4] (Srinivasan et al., 2004). Various tetrathio- tungstates with organic ammonium counter cations were characterized by Srinivasanet al.(2007).
Experimental Crystal data Cs2[WS4] Mr= 577.91 Orthorhombic,Pnma a= 10.0579 (9) A˚ b= 7.2362 (5) A˚ c= 12.7740 (9) A˚
V= 929.70 (12) A˚3 Z= 4
MoKradiation = 20.95 mm1 T= 170 (2) K 0.080.070.04 mm Data collection
Stoe IPDSI diffractometer Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1998) Tmin= 0.211,Tmax= 0.442
11509 measured reflections 1492 independent reflections 1322 reflections withI> 2(I) Rint= 0.060
Refinement
R[F2> 2(F2)] = 0.027 wR(F2) = 0.069 S= 1.03 1492 reflections
41 parameters max= 2.31 e A˚3 min=2.62 e A˚3
Table 1
Selected geometric parameters (A˚ ,).
W1—S3 2.1915 (12)
W1—S3i 2.1915 (12)
W1—S1 2.1935 (18)
W1—S2 2.2079 (18)
Cs1—S1ii 3.451 (2)
Cs1—S1 3.5331 (19)
Cs1—S3iii 3.5502 (14)
Cs1—S3iv 3.5502 (14)
Cs1—S3v 3.5680 (14)
Cs1—S3vi 3.5680 (14)
Cs1—S2ii 3.579 (2)
Cs1—S2iv 3.7072 (5)
Cs1—S2vii 3.7072 (5)
Cs2—S1viii 3.6564 (4)
Cs2—S1ix 3.6564 (4)
Cs2—S3x 3.7170 (15)
Cs2—S3viii 3.7170 (15)
Cs2—S3xi 3.7384 (14)
Cs2—S3xii 3.7384 (14)
Cs2—S2xiii 3.7527 (19)
Cs2—S2 3.926 (2)
Cs2—S3 4.0448 (16)
Cs2—S3i 4.0448 (16)
S3—W1—S3i 108.86 (7)
S3—W1—S1 108.92 (5)
S3—W1—S2 109.65 (4)
S1—W1—S2 110.82 (8)
Symmetry codes: (i) x;yþ12;z; (ii) x12;y;zþ12; (iii) xþ32;yþ12;z12; (iv) xþ32;y;z12; (v) xþ1;yþ12;zþ1; (vi) xþ1;y;zþ1; (vii) xþ32;yþ1;z12; (viii) xþ32;y;zþ12; (ix) xþ32;yþ1;zþ12; (x) xþ32;yþ12;zþ12; (xi) xþ12;yþ12;zþ32; (xii) xþ12;y;zþ32; (xiii) x12;y;zþ32.
Data collection:DIF4(Stoe & Cie, 1998); cell refinement:DIF4;
data reduction:REDU4(Stoe & Cie, 1998); program(s) used to solve structure: SHELXS97(Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics:
DIAMOND(Brandenburg, 1999); software used to prepare material for publication:XCIFinSHELXTL(Bruker, 1998).
This work was supported by the Department of Science and Technology (DST), New Delhi, under grant No. SR/S1/IC-41/
2003. BRS and WB thank the DST and the Deutscher Akademischer Austauschdienst (DAAD), Bonn, for the sanction of a DST–DAAD (PPP) project.
Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2130).
References
Brandenburg, K. (1999). DIAMOND. Version 2.1c. Crystal Impact GbR, Bonn, Germany.
Bruker (1998). SHELXTL. Version 5.10. Bruker AXS Inc., Madison, Wisconsin, USA.
Ellermeier, J., Na¨ther, C. & Bensch, W. (1999).Acta Cryst.C55, 1748–1751.
Emirdag-Eanes, M. & Ibers, J. A. (2001).Z. Kristallogr. New Cryst. Struct.216, 484.
Mu¨ller, A. & Sievert, W. (1974).Z. Anorg. Allg. Chem.403, 251–266.
Raymond, C. C., Dorhout, P. K. & Miller, S. M. (1995).Z. Kristallogr.210, 775.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Go¨ttingen, Germany.
Srinivasan, B. R., Naik, A. R., Na¨ther, C. & Bensch, W. (2007).Z. Anorg. Allg.
Chem.633, 582–588.
Srinivasan, B. R., Poisot, M., Na¨ther, C. & Bensch, W. (2004).Acta Cryst.E60, i136–i138.
Stoe & Cie (1998).DIF4(Version 7.09X/DOS),REDU4(Version 7.03) andX- SHAPE(Version 1.03). Stoe & Cie, Darmstadt, Germany.
Yao, J. & Ibers, J. A. (2004).Acta Cryst.E60, i10–i11.
inorganic compounds
Acta Crystallographica Section E
Structure Reports Online
ISSN 1600-5368
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