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Volume 69 
Part 12 
Pages m637-m638  
December 2013  

Received 23 September 2013
Accepted 21 October 2013
Online 6 November 2013

Key indicators
Single-crystal X-ray study
T = 298 K
Mean [sigma](C-C) = 0.008 Å
Disorder in main residue
R = 0.047
wR = 0.089
Data-to-parameter ratio = 37.1
Details
Open access

catena-Poly[N,N,N',N'-tetra­methyl­ethylendi­ammonium [[tetra­bromido­antimonate(III)]-[mu]-bromido] hemihydrate]

aLaboratoire de Génie des Matériaux et Environnement, Ecole Nationale d'Ingénieurs de Sfax, Université de Sfax, BP 1173, Sfax, Tunisia, and bService commun d'analyse par diffraction des rayons X, Université de Brest, 6 avenue Victor Le Gorgeu, CS 93837, F-29238 Brest Cedex 3, France
Correspondence e-mail: kharrat_houda@yahoo.fr

The asymmetric unit of the title compound {(C6H18N2)2[Sb2Br10]·H2O}n, consists of two tetra­methyl­ethylendi­ammonium cations that are located on centres of inversion, as well as one tetra­methyl­ethylendi­ammonium cation, one water mol­ecule, one distorted octahedral [SbBr6]3-anion and one bisphenoidal [SbBr4]- anion in general positions. The [SbBr6]3- and [SbBr4]- anions are linked together by two long Sb-Br bonds of 3.2709 (8) and 3.5447 (7) Å into {[Sb2Br10]4-}n chains along [001]. One of the three tetra­methyl­ethylendi­ammonium cations is disordered and was refined using a split model (occupancy ratio 0.58:0.42). The cations and the water mol­ecule are connected to the {[Sb2Br10]4-}n polymeric anions by weak N-H ...Br and O(water)-H ...Br hydrogen bonding.

Related literature

For crystal structures of related organic anti­monate(III) halogenides, see: Bujak & Angel (2005[Bujak, M. & Angel, R. J. (2005). J. Solid State Chem. 178, 2237-2246.]); Chaabouni et al. (1997[Chaabouni, S., Kamoun, S., Daoud, A. & Jouini, T. (1997). J. Chem. Crystallogr. 27, 401-404.], 1998[Chaabouni, S., Kamoun, S. & Jaud, J. (1998). Mater. Res. Bull. 33, 377-388.]). For a similar structure, see: Owczarek et al. (2012[Owczarek, M., Szklarz, P., Jakubas, R. & Miniewicz, A. (2012). Dalton Trans. 41, 7285-7294.]). The bond-valence sum was calculated using the parameters given by Brown & Altermatt (1985[Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.]).

[Scheme 1]

Experimental

Crystal data
  • (C6H18N2)[Sb2Br10]·H2O

  • Mr = 1297.06

  • Orthorhombic, P b c a

  • a = 18.0860 (4) Å

  • b = 19.1755 (4) Å

  • c = 19.4619 (4) Å

  • V = 6749.5 (2) Å3

  • Z = 8

  • Mo K[alpha] radiation

  • [mu] = 13.45 mm-1

  • T = 298 K

  • 0.43 × 0.30 × 0.19 mm

Data collection
  • Oxford Diffraction Xcalibur Sapphire2 diffractometer

  • Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2009[Oxford Diffraction (2009). CrystAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]) Tmin = 0.011, Tmax = 0.078

  • 65748 measured reflections

  • 10770 independent reflections

  • 5721 reflections with I > 2[sigma](I)

  • Rint = 0.096

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

  • wR(F2) = 0.089

  • S = 1.01

  • 10770 reflections

  • 290 parameters

  • 15 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 1.92 e Å-3

  • [Delta][rho]min = -1.98 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N1-H1...Br1 0.91 2.59 3.362 (4) 143
N2-H2...Br1 0.91 2.56 3.353 (5) 146
N3-H3...Br7i 0.91 2.5 3.352 (4) 157
N4-H4...Br3 0.91 2.52 3.318 (4) 147
OW-H1W...Br4ii 0.83 3.03 3.759 (7) 148
OW-H2W...Br3 0.83 2.67 3.449 (7) 157
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) [x-{\script{1\over 2}}, -y+{\script{3\over 2}}, -z+1].

Data collection: CrysAlis CCD (Oxford Diffraction, 2009[Oxford Diffraction (2009). CrystAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]); cell refinement: CrysAlis RED (Oxford Diffraction, 2009[Oxford Diffraction (2009). CrystAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]); data reduction: CrysAlis RED; program(s) used to solve structure: SIR92 (Altomare et al., 1993[Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993). J. Appl. Cryst. 26, 343-350.]); 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.]) and Mercury (Macrae et al., 2008[Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470.]); software used to prepare material for publication: WinGX (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]) 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: NC2318 ).


Acknowledgements

The authors gratefully acknowledge the support of the Tunisian Ministry of Higher Education and Scientific Research.

References

Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993). J. Appl. Cryst. 26, 343-350.  [CrossRef] [Web of Science] [IUCr Journals]
Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.  [CrossRef] [Web of Science] [IUCr Journals]
Bujak, M. & Angel, R. J. (2005). J. Solid State Chem. 178, 2237-2246.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Chaabouni, S., Kamoun, S., Daoud, A. & Jouini, T. (1997). J. Chem. Crystallogr. 27, 401-404.  [CrossRef] [ChemPort]
Chaabouni, S., Kamoun, S. & Jaud, J. (1998). Mater. Res. Bull. 33, 377-388.  [Web of Science] [CrossRef] [ChemPort]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Owczarek, M., Szklarz, P., Jakubas, R. & Miniewicz, A. (2012). Dalton Trans. 41, 7285-7294.  [CSD] [CrossRef] [ChemPort] [PubMed]
Oxford Diffraction (2009). CrystAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]


Acta Cryst (2013). E69, m637-m638   [ doi:10.1107/S1600536813028894 ]

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