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Volume 69 
Part 12 
Page m689  
December 2013  

Received 20 November 2013
Accepted 25 November 2013
Online 30 November 2013

Key indicators
Single-crystal X-ray study
T = 223 K
Mean [sigma](C-C) = 0.007 Å
R = 0.047
wR = 0.074
Data-to-parameter ratio = 12.8
Details
Open access

[mu]-Hexa­thio­metadiphosphato-bis­[(1,4,7,10,13,16-hexa­oxa­cyclo­octa­decane-[kappa]6O)rubidium] aceto­nitrile disolvate

aInstitute of Inorganic and Analytical Chemistry, Clausthal University of Technology, Paul-Ernst-Strasse 4, D-38678 Clausthal-Zellerfeld, Germany, and bChemistry Department, University of Vlora, Sheshi Pavaresia, 9401 Vlore, Albania
Correspondence e-mail: mimoza.gjikaj@tu-clausthal.de

The asymmetric unit of the title compound, [Rb2(P2S6)(C12H24O6)2]·2CH3CN, contains one half of an [Rb(18-crown-6)2]2[P2S6] unit and one aceto­nitrile solvent mol­ecule. The [Rb(18-crown-6)]2[P2S6] unit is completed by inversion symmetry. Its Rb+ ion is situated near the centre of the macrocyclic cavity, but is displaced by 0.8972 (1) Å from the O atoms of the crown in the direction of the [P2S6]2- moiety. The overall coordination number of the cation is eight, defined by the six crown ether O atoms and by two terminal S atoms of the [P2S6]2- anion. The hexa­thio­metadiphosphate anion is built up from two tetra­hedral PS4 units joined together by a common edge. The crystal structure is characterized by alternating layers of [Rb(18-crown-6)]2[P2S6] and aceto­nitrile solvent mol­ecules stacked along [010].

Related literature

For the synthesis of hexa­thio­metadiphosphates, see: Thilo & Ladwig (1962[Thilo, E. & Ladwig, G. (1962). Monatsber. Dtsch Akad. Wiss. Berlin, 4, 720-724.]). For the crystal structures of hexa­thio­metadiphosphates, see: Toffoli et al. (1978[Toffoli, P., Khodadad, P. & Rodier, N. (1978). Acta Cryst. B34, 3561-3564.]); Brockner et al. (1985[Brockner, W., Becker, R., Eisenmann, B. & Schäfer, H. (1985). Z. Anorg. Allg. Chem. 520, 51-58.]). For the crystal structures of alkali crown ether hexa­thio­metadiphosphates, see: Gjikaj et al. (2005[Gjikaj, M., Adam, A., Duewel, M. & Brockner, W. (2005). Z. Kristallogr. New Cryst. Struct. 220, 67.], 2006[Gjikaj, M., Adam, A. & Brockner, W. (2006). Z. Anorg. Allg. Chem. 632, 279-283.]).

[Scheme 1]

Experimental

Crystal data
  • [Rb2(P2S6)(C12H24O6)2]·2C2H3N

  • Mr = 1035.98

  • Monoclinic, P 21 /c

  • a = 8.2261 (9) Å

  • b = 17.1054 (15) Å

  • c = 16.5895 (18) Å

  • [beta] = 95.520 (9)°

  • V = 2323.5 (4) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 2.50 mm-1

  • T = 223 K

  • 0.29 × 0.26 × 0.22 mm

Data collection
  • Stoe IPDSII diffractometer

  • Absorption correction: numerical (X-SHAPE and X-RED; Stoe & Cie, 1999[Stoe & Cie (1999). X-SHAPE. Stoe & Cie GmbH, Darmstadt, Germany.], 2001[Stoe & Cie (2001). X-RED. Stoe & Cie GmbH, Darmstadt, Germany.]) Tmin = 0.490, Tmax = 0.577

  • 26056 measured reflections

  • 4400 independent reflections

  • 3450 reflections with I > 2[sigma](I)

  • Rint = 0.092

Refinement
  • R[F2 > 2[sigma](F2)] = 0.047

  • wR(F2) = 0.074

  • S = 1.15

  • 4400 reflections

  • 343 parameters

  • All H-atom parameters refined

  • [Delta][rho]max = 0.50 e Å-3

  • [Delta][rho]min = -0.28 e Å-3

Data collection: X-AREA (Stoe & Cie, 2002[Stoe & Cie (2002). X-AREA. Stoe & Cie GmbH, Darmstadt, Germany.]); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]); software used to prepare material for publication: SHELXL97, PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]) and publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2785 ).


References

Brockner, W., Becker, R., Eisenmann, B. & Schäfer, H. (1985). Z. Anorg. Allg. Chem. 520, 51-58.  [CrossRef] [ChemPort]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Gjikaj, M., Adam, A. & Brockner, W. (2006). Z. Anorg. Allg. Chem. 632, 279-283.  [CrossRef] [ChemPort]
Gjikaj, M., Adam, A., Duewel, M. & Brockner, W. (2005). Z. Kristallogr. New Cryst. Struct. 220, 67.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Spek, A. L. (2009). Acta Cryst. D65, 148-155.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Stoe & Cie (1999). X-SHAPE. Stoe & Cie GmbH, Darmstadt, Germany.
Stoe & Cie (2001). X-RED. Stoe & Cie GmbH, Darmstadt, Germany.
Stoe & Cie (2002). X-AREA. Stoe & Cie GmbH, Darmstadt, Germany.
Thilo, E. & Ladwig, G. (1962). Monatsber. Dtsch Akad. Wiss. Berlin, 4, 720-724.  [ChemPort]
Toffoli, P., Khodadad, P. & Rodier, N. (1978). Acta Cryst. B34, 3561-3564.  [CrossRef] [IUCr Journals]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]


Acta Cryst (2013). E69, m689  [ doi:10.1107/S1600536813032121 ]

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