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Volume 68 
Part 12 
Pages m1437-m1438  
December 2012  

Received 10 August 2012
Accepted 14 October 2012
Online 3 November 2012

Key indicators
Single-crystal X-ray study
T = 200 K
Mean [sigma](C-C) = 0.007 Å
R = 0.032
wR = 0.078
Data-to-parameter ratio = 17.9
Details
Open access

catena-Poly[[[dichlorido(pyridin-1-ium-3-yl)arsenic(III)]-[mu]-chlorido] monohydrate]

aSchool of Chemistry, Trinity College Dublin, Dublin 2, Ireland
Correspondence e-mail: schmittw@tcd.ie

The crystal structure of the title compound, {[AsCl3(C5H5N)]·H2O}n, is characterized by polymeric chains consisting of alternating arsenic and chlorine atoms running parallel to the a axis. O-H...Cl and N-H...O hydrogen bonds mediated by non-coordinating water molecules assemble these chains into a three-dimensional framework. The AsIII atom, the atoms of the pyridinium ring and the water O atom have m site symmetry and the bridging Cl atom has site symmetry 2. This is the first reported organotrichloroarsenate(III) in which arsenic adopts a [psi]-octahedral fivefold coordination.

Related literature

For the synthesis, see: Binz & von Schickh (1936[Binz, A. & von Schickh, O. (1936). German Patent DE 633867.]). For monomeric and oligomeric monoorganohaloarsenates(III) with tetracoordinate arsenic, see: Grewe et al. (1998[Grewe, S., Häusler, T., Mannel, M., Rossenbeck, B. & Sheldrick, W. S. (1998). Z. Anorg. Allg. Chem. 624, 613-619.]). For homologous monoorganohaloantimonate(III)/-bismuthate(III) structures, see: Althaus et al. (1999[Althaus, H., Breunig, H. J. & Lork, E. (1999). Chem. Commun. pp. 1971-1972.]); Breunig et al. (1992[Breunig, H. J., Ebert, K. H., Gülec, S., Dräger, M., Sowerby, D. B., Begley, M. J. & Behrens, U. (1992). J. Organomet. Chem. 427, 39-48.], 1999[Breunig, H. J., Denker, M. & Lork, E. (1999). Z. Anorg. Allg. Chem. 625, 117-120.], 2010[Breunig, H. J., Koehne, T., Lork, E., Moldovan, O., Poveleit, J. & Rat, C. I. (2010). Z. Naturforsch. Teil B, 65, 1245-1248.]); Hall & Sowerby (1988[Hall, M. & Sowerby, D. B. (1988). J. Organomet. Chem. 347, 59-70.]); James et al. (1999[James, S. C., Norman, N. C. & Orpen, A. G. (1999). J. Chem. Soc. Dalton Trans. pp. 2837-2843.]); Preut et al. (1987[Preut, H., Huber, F. & Alonzo, G. (1987). Acta Cryst. C43, 46-48.]); Sheldrick & Martin (1992[Sheldrick, W. S. & Martin, C. (1992). Z. Naturforsch. Teil B, 47, 919-924.]); von Seyerl et al. (1986[Seyerl, J. von, Scheidsteger, O., Berke, H. & Huttner, G. (1986). J. Organomet. Chem. 311, 85-89.]). For organoarsenic functionalized metal oxide clusters, see: Breen, Clérac et al. (2012[Breen, J. M., Clérac, R., Zhang, L., Cloonan, S. M., Kennedy, E., Feeney, M., McCabe, T., Willams, D. C. & Schmitt, W. (2012). Dalton Trans. 41, 2918-2926.]); Breen, Zhang et al. (2012[Breen, J. M., Zhang, L., Clement, R. & Schmitt, W. (2012). Inorg. Chem. 51, 19-21.]); Onet et al. (2011[Onet, C. I., Zhang, L., Clérac, R., Jean-Denis, J. B., Feeney, M., McCabe, T. & Schmitt, W. (2011). Inorg. Chem. 50, 604-613.]); Zhang et al. (2012[Zhang, L., Clérac, R., Heijboer, P. & Schmitt, W. (2012). Angew. Chem. Int. Ed. 51, 3007-3011.]).

[Scheme 1]

Experimental

Crystal data
  • [AsCl3(C5H5N)]·H2O

  • Mr = 278.39

  • Orthorhombic, I m 2a

  • a = 8.2107 (9) Å

  • b = 8.5812 (9) Å

  • c = 13.2046 (14) Å

  • V = 930.37 (17) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 4.46 mm-1

  • T = 200 K

  • 0.5 × 0.2 × 0.2 mm

Data collection
  • Bruker SMART APEX CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 1997[Bruker (1997). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.341, Tmax = 0.469

  • 3423 measured reflections

  • 1184 independent reflections

  • 1167 reflections with I > 2[sigma](I)

  • Rint = 0.068

Refinement
  • R[F2 > 2[sigma](F2)] = 0.032

  • wR(F2) = 0.078

  • S = 1.10

  • 1184 reflections

  • 66 parameters

  • 3 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • [Delta][rho]max = 1.14 e Å-3

  • [Delta][rho]min = -1.28 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 529 Friedel pairs

  • Flack parameter: 0.006 (12)

Table 1
Selected bond lengths (Å)

As1-Cl1 2.2624 (8)
As1-Cl2 2.8907 (5)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O1-H1...Cl2 0.82 (2) 2.40 (2) 3.197 (2) 165 (3)
N3-H3...O1i 0.88 1.84 2.711 173
Symmetry code: (i) [-x+{\script{3\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}].

Data collection: SMART (Bruker, 1997[Bruker (1997). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 1997[Bruker (1997). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; 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: OLEX2 (Dolomanov et al., 2009[Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.]); software used to prepare material for publication: OLEX2.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NK2180 ).


Acknowledgements

The authors thank the Science Foundation Ireland (SFI,06/RFP/CHE173 and 08/IN.1/I2047)for financial support.

References

Althaus, H., Breunig, H. J. & Lork, E. (1999). Chem. Commun. pp. 1971-1972.  [CSD] [CrossRef]
Binz, A. & von Schickh, O. (1936). German Patent DE 633867.
Breen, J. M., Clérac, R., Zhang, L., Cloonan, S. M., Kennedy, E., Feeney, M., McCabe, T., Willams, D. C. & Schmitt, W. (2012). Dalton Trans. 41, 2918-2926.  [CSD] [CrossRef] [ChemPort] [PubMed]
Breen, J. M., Zhang, L., Clement, R. & Schmitt, W. (2012). Inorg. Chem. 51, 19-21.  [ISI] [CSD] [CrossRef] [ChemPort] [PubMed]
Breunig, H. J., Denker, M. & Lork, E. (1999). Z. Anorg. Allg. Chem. 625, 117-120.  [CrossRef] [ChemPort]
Breunig, H. J., Ebert, K. H., Gülec, S., Dräger, M., Sowerby, D. B., Begley, M. J. & Behrens, U. (1992). J. Organomet. Chem. 427, 39-48.  [CrossRef] [ChemPort]
Breunig, H. J., Koehne, T., Lork, E., Moldovan, O., Poveleit, J. & Rat, C. I. (2010). Z. Naturforsch. Teil B, 65, 1245-1248.  [ChemPort]
Bruker (1997). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.  [ISI] [CrossRef] [ChemPort] [details]
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Grewe, S., Häusler, T., Mannel, M., Rossenbeck, B. & Sheldrick, W. S. (1998). Z. Anorg. Allg. Chem. 624, 613-619.  [CrossRef] [ChemPort]
Hall, M. & Sowerby, D. B. (1988). J. Organomet. Chem. 347, 59-70.  [CrossRef] [ChemPort]
James, S. C., Norman, N. C. & Orpen, A. G. (1999). J. Chem. Soc. Dalton Trans. pp. 2837-2843.  [CSD] [CrossRef]
Onet, C. I., Zhang, L., Clérac, R., Jean-Denis, J. B., Feeney, M., McCabe, T. & Schmitt, W. (2011). Inorg. Chem. 50, 604-613.  [ISI] [CSD] [CrossRef] [ChemPort]
Preut, H., Huber, F. & Alonzo, G. (1987). Acta Cryst. C43, 46-48.  [CrossRef] [details]
Seyerl, J. von, Scheidsteger, O., Berke, H. & Huttner, G. (1986). J. Organomet. Chem. 311, 85-89.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Sheldrick, W. S. & Martin, C. (1992). Z. Naturforsch. Teil B, 47, 919-924.  [ChemPort]
Zhang, L., Clérac, R., Heijboer, P. & Schmitt, W. (2012). Angew. Chem. Int. Ed. 51, 3007-3011.  [ChemPort]


Acta Cryst (2012). E68, m1437-m1438   [ doi:10.1107/S1600536812042882 ]

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