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Volume 69 
Part 6 
Page i37  
June 2013  

Received 7 May 2013
Accepted 17 May 2013
Online 25 May 2013

Key indicators
Single-crystal X-ray study
T = 298 K
Mean [sigma](As-O) = 0.004 Å
R = 0.018
wR = 0.045
Data-to-parameter ratio = 13.9
Details
Open access

K(MoO2)4O3(AsO4)

aLaboratoire de Matériaux et Cristallochimie, Faculté des Sciences de Tunis, Université de Tunis ElManar, 2092 ElManar II Tunis, Tunisia
Correspondence e-mail: faouzi.zid@fst.rnu.tn

A new compound with a non-centrosymmetric structure, potassium tetrakis[dioxomolybdenum(IV)] arsenate trioxide, K(MoO2)4O3(AsO4), has been synthesized by a solid-state reaction. The [(MoO2)4O3(AsO4)]+ three-dimensional framework consists of single arsenate AsO4 tetrahedra, MoO6 octahedra, MoO5 bipyramids and bioctahedral units of edge-sharing Mo2O10 octahedra. The [Mo2O8][infinity] octahedral chains running along the a-axis direction are connected through their corners to the AsO4 tetrahedra, MoO6 octahedra and MoO5 bipyramids, so as to form large tunnels propagating along the a axis in which the K+ cations are located. This structure is compared with compounds containing M2O10 (M = Mo, V, Fe) dimers and with those containing M2O8 (M = V) chains.

Related literature

For background to the physico-chemical properties of related compounds, see: Piffard et al. (1985[Piffard, Y., Lachgar, A. & Tournoux, M. (1985). J. Solid State Chem. 109, 253-256.]); Centi et al. (1988[Centi, G., Trifiro, F., Ebner, J. R. & Franchetti, V. M. (1988). Chem. Rev. 88, 55-80.]); Stucky et al. (1989[Stucky, G. D., Phillips, M. L. F. & Gier, T. E. (1989). Chem. Mater. 1, 492-509.]); Northrup et al. (1994[Northrup, P. A., Parise, J. B., Cheng, L. K., Cheng, L. T. & McCarron, E. M. (1994). Chem. Mater. 6, 434-440.]); Ouerfelli et al. (2007[Ouerfelli, N., Guesmi, A., Molinié, P., Mazza, D., Zid, M. F. & Driss, A. (2007). J. Solid State Chem. 180, 2942-2949.]). For details of structurally related compounds, see: Amoros & LeBail (1992[Amoros, P. & LeBail, A. (1992). J. Solid State Chem. 97, 283-291.]), Boudin et al. (1994[Boudin, S., Grandin, A., Borel, M. M., Leclaire, A. & Raveau, B. (1994). J. Solid State Chem. 110, 43-49.]); Guesdon et al. (1994[Guesdon, A., Borel, M. M., Leclaire, A., Grandin, A. & Raveau, B. (1994). J. Solid State Chem. 109, 145-151.], 1995[Guesdon, A., Leclaire, A., Borel, M. M., Grandin, A. & Raveau, B. (1995). J. Solid State Chem. 114, 481-485.]); Borel et al. (1994[Borel, M. M., Guesdon, A., Leclaire, A., Grandin, A. & Raveau, B. (1994). Z. Anorg. Allg. Chem. 620, 569-573.], 2000[Borel, M. M., Leclaire, A., Chardon, J. & Raveau, B. (2000). Int. J. Inorg. Mater. 2, 11-19.]); LeBail et al. (1995[LeBail, A., Permier, L. & Laligant, Y. (1995). Eur. J. Solid State Inorg. Chem. 32, 883-892.]); Berrah et al. (1999[Berrah, F., Borel, M. M., Leclaire, A., Daturi, M. & Raveau, B. (1999). J. Solid State Chem. 145, 643-648.]); Hajji et al. (2009[Hajji, M., Zid, M. F. & Driss, A. (2009). Acta Cryst. E65, i21.]). For the preparation, see: Jouini et al. (2012[Jouini, R., Zid, M. F. & Driss, A. (2012). Acta Cryst. E68, i93.]). For bond-valence sums, see: Brown & Altermatt (1985[Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.]).

Experimental

Crystal data
  • K(MoO2)4O3(AsO4)

  • Mr = 737.78

  • Orthorhombic, P 21 21 21

  • a = 8.0442 (8) Å

  • b = 11.9167 (9) Å

  • c = 12.6799 (10) Å

  • V = 1215.50 (18) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 7.16 mm-1

  • T = 298 K

  • 0.42 × 0.33 × 0.22 mm

Data collection
  • Enraf-Nonius CAD-4 diffractometer

  • Absorption correction: [psi] scan (North et al., 1968[North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359.]) Tmin = 0.077, Tmax = 0.212

  • 8046 measured reflections

  • 2647 independent reflections

  • 2611 reflections with I > 2[sigma](I)

  • Rint = 0.030

  • 2 standard reflections every 120 min intensity decay: 1.2%

Refinement
  • R[F2 > 2[sigma](F2)] = 0.018

  • wR(F2) = 0.045

  • S = 1.10

  • 2647 reflections

  • 191 parameters

  • [Delta][rho]max = 0.52 e Å-3

  • [Delta][rho]min = -0.69 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 2399 Friedel pairs

  • Flack parameter: 0.089 (10)

Data collection: CAD-4 EXPRESS (Duisenberg, 1992[Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96.]; Macícek & Yordanov, 1992[Macícek, J. & Yordanov, A. (1992). J. Appl. Cryst. 25, 73-80.]); cell refinement: CAD-4 EXPRESS); data reduction: XCAD4 (Harms & Wocadlo, 1995[Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany.]); 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: DIAMOND (Brandenburg, 1998[Brandenburg, K. (1998). Diamond. University of Bonn, Germany.]); software used to prepare material for publication: WinGX (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: VN2070 ).


References

Amoros, P. & LeBail, A. (1992). J. Solid State Chem. 97, 283-291.  [CrossRef] [ChemPort] [ISI]
Berrah, F., Borel, M. M., Leclaire, A., Daturi, M. & Raveau, B. (1999). J. Solid State Chem. 145, 643-648.  [ISI] [CrossRef] [ChemPort]
Borel, M. M., Guesdon, A., Leclaire, A., Grandin, A. & Raveau, B. (1994). Z. Anorg. Allg. Chem. 620, 569-573.  [CrossRef] [ChemPort]
Borel, M. M., Leclaire, A., Chardon, J. & Raveau, B. (2000). Int. J. Inorg. Mater. 2, 11-19.  [ISI] [CrossRef] [ChemPort]
Boudin, S., Grandin, A., Borel, M. M., Leclaire, A. & Raveau, B. (1994). J. Solid State Chem. 110, 43-49.  [CrossRef] [ChemPort] [ISI]
Brandenburg, K. (1998). Diamond. University of Bonn, Germany.
Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.  [CrossRef] [ISI] [details]
Centi, G., Trifiro, F., Ebner, J. R. & Franchetti, V. M. (1988). Chem. Rev. 88, 55-80.  [CrossRef] [ChemPort] [ISI]
Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96.  [CrossRef] [ChemPort] [ISI] [details]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Guesdon, A., Borel, M. M., Leclaire, A., Grandin, A. & Raveau, B. (1994). J. Solid State Chem. 109, 145-151.  [CrossRef] [ChemPort] [ISI]
Guesdon, A., Leclaire, A., Borel, M. M., Grandin, A. & Raveau, B. (1995). J. Solid State Chem. 114, 481-485.  [CrossRef] [ChemPort] [ISI]
Hajji, M., Zid, M. F. & Driss, A. (2009). Acta Cryst. E65, i21.  [CrossRef] [details]
Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany.
Jouini, R., Zid, M. F. & Driss, A. (2012). Acta Cryst. E68, i93.  [CrossRef] [details]
LeBail, A., Permier, L. & Laligant, Y. (1995). Eur. J. Solid State Inorg. Chem. 32, 883-892.  [ChemPort]
Macícek, J. & Yordanov, A. (1992). J. Appl. Cryst. 25, 73-80.  [CrossRef] [ISI] [details]
North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359.  [CrossRef] [details]
Northrup, P. A., Parise, J. B., Cheng, L. K., Cheng, L. T. & McCarron, E. M. (1994). Chem. Mater. 6, 434-440.  [CrossRef] [ChemPort] [ISI]
Ouerfelli, N., Guesmi, A., Molinié, P., Mazza, D., Zid, M. F. & Driss, A. (2007). J. Solid State Chem. 180, 2942-2949.  [ISI] [CrossRef] [ChemPort]
Piffard, Y., Lachgar, A. & Tournoux, M. (1985). J. Solid State Chem. 109, 253-256.  [CrossRef] [ISI]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [details]
Stucky, G. D., Phillips, M. L. F. & Gier, T. E. (1989). Chem. Mater. 1, 492-509.  [CrossRef] [ChemPort]


Acta Cryst (2013). E69, i37  [ doi:10.1107/S1600536813013664 ]

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