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Volume 69 
Part 10 
Pages i67-i68  
October 2013  

Received 26 August 2013
Accepted 19 September 2013
Online 25 September 2013

Key indicators
Single-crystal X-ray study
T = 293 K
Mean [sigma](Mo-Se) = 0.001 Å
Disorder in solvent or counterion
R = 0.033
wR = 0.084
Data-to-parameter ratio = 37.1
Details
Open access

Na3.88Mo15Se19: a novel ternary reduced molybdenum selenide containing Mo6 and Mo9 clusters

aFaculty of Science III, Lebanese University, PO Box 826, Kobbeh-Tripoli, Lebanon, and bUnité Sciences Chimiques de Rennes, UMR CNRS No. 6226, Université de Rennes I - INSA Rennes, Campus de Beaulieu, 35042 Rennes CEDEX, France
Correspondence e-mail: Patrick.Gougeon@univ-rennes1.fr

The structure of tetrasodium pentadecamolybdenum nonadecaselenide, Na3.88Mo15Se19, is isotypic with the In3+xMo15Se19 compounds [Grüttner et al. (1979[Grüttner, A., Yvon, K., Chevrel, R., Potel, M., Sergent, M. & Seeber, B. (1979). Acta Cryst. B35, 285-292.]). Acta Cryst. B35, 285-292]. It is characterized by two cluster units, Mo6Sei8Sea6 and Mo9Sei11Sea6 (where i represents inner and a apical atoms), that are present in a 1:1 ratio. The cluster units are centered at Wyckoff positions 2b and 2c and have point-group symmetry -3 and -6, respectively. The clusters are interconnected through additional Mo-Se bonds. In the title compound, the Na+ cations replace the trivalent as well as the monovalent indium atoms present in In3.9Mo15Se19. One Mo, one Se and one Na atom are situated on mirror planes, and two other Se atoms and one Na atom [occupancy 0.628 (14)] are situated on threefold rotation axes. The crystal studied was twinned by merohedry with refined components of 0.4216 (12) and 0.5784 (12).

Related literature

For previous reports on the crystal structures of In3Mo15Se19 compounds, see: Grüttner et al. (1979[Grüttner, A., Yvon, K., Chevrel, R., Potel, M., Sergent, M. & Seeber, B. (1979). Acta Cryst. B35, 285-292.]). For physical properties of this type of compounds, see: Seeber et al. (1979[Seeber, B., Decroux, M., Fisher, Ø., Chevrel, R., Sergent, M. & Grüttner, A. (1979). Solid State Commun. 29, 419-423.]). The crystal structures of the substituted selenides Ho0.76In1.68Mo15Se19 and In0.87K2Mo15Se19 were reported by Salloum et al. (2006[Salloum, D., Gougeon, P. & Potel, M. (2006). Acta Cryst. E62, i83-i85.], 2007[Salloum, D., Gougeon, P. & Potel, M. (2007). Acta Cryst. E63, i8-i10.]). For the isotypic sulfides In3.7Mo15S19, In1.6Rb2Mo15S19, In2.2CsMo15S19 and ScTl2Mo15S19, see: Salloum et al. (2004a[Salloum, D., Gautier, R., Gougeon, P. & Potel, M. (2004a). J. Solid State Chem. 177, 1672-1680.],b[Salloum, D., Gougeon, P., Roisnel, T. & Potel, M. (2004b). J. Alloys Compd, 383, 57-62.]); Gougeon et al. (2010[Gougeon, P., Gall, P., Salloum, D. & Potel, M. (2010). Acta Cryst. E66, i73.]). For details of the i- and a-type ligand notation, see: Schäfer & von Schnering (1964[Schäfer, H. & von Schnering, H. G. (1964). Angew. Chem. 76, 833-845.]).

Experimental

Crystal data
  • Na3.88Mo15Se19

  • Mr = 3028.54

  • Hexagonal, P 63 /m

  • a = 9.8647 (1) Å

  • c = 19.5957 (3) Å

  • V = 1651.43 (3) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 26.47 mm-1

  • T = 293 K

  • 0.09 × 0.07 × 0.06 mm

Data collection
  • Nonius KappaCCD diffractometer

  • Absorption correction: analytical (de Meulenaer & Tompa, 1965[Meulenaer, J. de & Tompa, H. (1965). Acta Cryst. 19, 1014-1018.]) Tmin = 0.111, Tmax = 0.215

  • 25999 measured reflections

  • 2487 independent reflections

  • 2116 reflections with I > 2[sigma](I)

  • Rint = 0.075

Refinement
  • R[F2 > 2[sigma](F2)] = 0.033

  • wR(F2) = 0.084

  • S = 1.06

  • 2487 reflections

  • 67 parameters

  • [Delta][rho]max = 2.69 e Å-3

  • [Delta][rho]min = -1.81 e Å-3

Table 1
Selected bond lengths (Å)

Mo1-Se4i 2.5287 (7)
Mo1-Se1ii 2.5600 (6)
Mo1-Se1 2.5810 (7)
Mo1-Se1iii 2.6075 (7)
Mo1-Mo1iii 2.6980 (7)
Mo1-Mo1ii 2.7152 (7)
Mo1-Se2iv 2.7207 (7)
Mo2-Se5 2.5220 (7)
Mo2-Se2 2.6023 (8)
Mo2-Mo2v 2.6311 (7)
Mo2-Se2vi 2.6312 (8)
Mo2-Se3 2.6830 (6)
Mo2-Se1 2.7018 (7)
Mo2-Mo3vi 2.7153 (6)
Mo2-Mo3 2.7537 (6)
Mo3-Se3 2.5586 (11)
Mo3-Se3v 2.5675 (11)
Mo3-Se2 2.6153 (6)
Mo3-Se2vii 2.6153 (6)
Mo3-Mo3vi 2.6834 (11)
Se5-Na1 2.848 (6)
Na1-Se2viii 3.2010 (11)
Na1-Se1ix 3.462 (2)
Na2-Se3v 2.657 (5)
Na2-Se4vii 2.747 (4)
Na2-Se2x 2.812 (4)
Na2-Se3xi 3.096 (5)
Symmetry codes: (i) x+1, y, z; (ii) x-y, x-1, -z+1; (iii) -y+1, x-y-1, z; (iv) -x+y+1, -x, z; (v) -x+y+1, -x+1, z; (vi) -y+1, x-y, z; (vii) [x, y, -z+{\script{3\over 2}}]; (viii) -x+1, -y, -z+1; (ix) y+1, -x+y+1, -z+1; (x) [-y, x-y, -z+{\script{3\over 2}}]; (xi) x-1, y, z.

Data collection: COLLECT (Nonius, 1998[Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.]); cell refinement: COLLECT; data reduction: EVALCCD (Duisenberg, 1998[Duisenberg, A. J. M. (1998). PhD thesis, University of Utrecht, The Netherlands.]); program(s) used to solve structure: SIR97 (Altomare et al., 1999[Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Bergerhoff, 1996[Bergerhoff, G. (1996). DIAMOND. University of Bonn, Germany.]); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: RU2054 ).


Acknowledgements

Intensity data were collected on the Nonius KappaCCD X-ray diffactometer system of the Centre de diffractométrie de l'Université de Rennes I (www.cdifx.univ-rennes1.fr).

References

Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Bergerhoff, G. (1996). DIAMOND. University of Bonn, Germany.
Duisenberg, A. J. M. (1998). PhD thesis, University of Utrecht, The Netherlands.
Gougeon, P., Gall, P., Salloum, D. & Potel, M. (2010). Acta Cryst. E66, i73.  [CrossRef] [IUCr Journals]
Grüttner, A., Yvon, K., Chevrel, R., Potel, M., Sergent, M. & Seeber, B. (1979). Acta Cryst. B35, 285-292.  [CrossRef] [IUCr Journals] [Web of Science]
Meulenaer, J. de & Tompa, H. (1965). Acta Cryst. 19, 1014-1018.  [CrossRef] [IUCr Journals]
Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.
Salloum, D., Gautier, R., Gougeon, P. & Potel, M. (2004a). J. Solid State Chem. 177, 1672-1680.  [Web of Science] [CrossRef] [ChemPort]
Salloum, D., Gougeon, P. & Potel, M. (2006). Acta Cryst. E62, i83-i85.  [CrossRef] [ChemPort] [IUCr Journals]
Salloum, D., Gougeon, P. & Potel, M. (2007). Acta Cryst. E63, i8-i10.  [CrossRef] [ChemPort] [IUCr Journals]
Salloum, D., Gougeon, P., Roisnel, T. & Potel, M. (2004b). J. Alloys Compd, 383, 57-62.  [Web of Science] [CrossRef] [ChemPort]
Schäfer, H. & von Schnering, H. G. (1964). Angew. Chem. 76, 833-845.
Seeber, B., Decroux, M., Fisher, Ø., Chevrel, R., Sergent, M. & Grüttner, A. (1979). Solid State Commun. 29, 419-423.  [CrossRef] [ChemPort] [Web of Science]
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]


Acta Cryst (2013). E69, i67-i68   [ doi:10.1107/S1600536813025907 ]

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