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

Reck, L.; Schmitt, W.

doi:10.1107/S1600536812042882

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 (C-C) = 0.007 Å
R = 0.032
wR = 0.078
Data-to-parameter ratio = 17.9
Details

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

Lukas Reck ^a and Wolfgang Schmitt ^a ^*

^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-HCl and N-HO hydrogen bonds mediated by non-coordinating water molecules assemble these chains into a three-dimensional framework. The As^III 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). For monomeric and oligomeric monoorganohaloarsenates(III) with tetracoordinate arsenic, see: Grewe et al. (1998). For homologous monoorganohaloantimonate(III)/-bismuthate(III) structures, see: Althaus et al. (1999); Breunig et al. (1992, 1999, 2010); Hall & Sowerby (1988); James et al. (1999); Preut et al. (1987); Sheldrick & Martin (1992); von Seyerl et al. (1986). For organoarsenic functionalized metal oxide clusters, see: Breen, Clérac et al. (2012); Breen, Zhang et al. (2012); Onet et al. (2011); Zhang et al. (2012).

Experimental

Crystal data

[AsCl₃(C₅H₅N)]·H₂O
M_r = 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 radiation
= 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) T_min = 0.341, T_max = 0.469
3423 measured reflections
1184 independent reflections
1167 reflections with I > 2(I)
R_int = 0.068

Refinement

R[F² > 2(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
_max = 1.14 e Å^-3
_min = -1.28 e Å^-3
Absolute structure: Flack (1983), 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-HA	D-H	HA	DA	D-HA
O1-H1Cl2	0.82 (2)	2.40 (2)	3.197 (2)	165 (3)
N3-H3O1ⁱ	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); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: OLEX2 (Dolomanov et al., 2009); 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

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metal-organic compounds