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Volume 69 
Part 7 
Page m353  
July 2013  

Received 15 May 2013
Accepted 23 May 2013
Online 8 June 2013

Key indicators
Single-crystal X-ray study
T = 296 K
Mean [sigma](C-C) = 0.011 Å
Disorder in main residue
R = 0.042
wR = 0.096
Data-to-parameter ratio = 30.3
Details
Open access

Tris(N,N-dimethylanilinium) tri-[mu]-bromido-bis[tribromidoantimonate(III)]

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

In the title compound, (C8H12N)3[Sb2Br9], two of the three unique N,N-dimethyanilinium cations exhibit flip-flop disorder with an occupancy ratio of 0.58 (1):0.42 (1). N-H...Br hydrogen bonds link the organic cations and bioctahedral face-sharing anions into a three-dimensional network.

Related literature

For related hybrid organic antimonate(III) halogenide crystal structures, 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 dielectric and phase transitions properties, see: Chaabouni & Kamoun (1998[Chaabouni, S. & Kamoun, S. (1998). Phase Transitions, 66, 119-127.]).

[Scheme 1]

Experimental

Crystal data
  • (C8H12N)3[Sb2Br9]

  • Mr = 1329.25

  • Triclinic, [P \overline 1]

  • a = 9.7857 (3) Å

  • b = 13.7658 (5) Å

  • c = 17.0297 (6) Å

  • [alpha] = 66.581 (4)°

  • [beta] = 78.689 (3)°

  • [gamma] = 72.601 (3)°

  • V = 2000.91 (14) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 10.36 mm-1

  • T = 296 K

  • 0.58 × 0.29 × 0.20 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, Oxfordshire, England.]) Tmin = 0.038, Tmax = 0.126

  • 29905 measured reflections

  • 12050 independent reflections

  • 6232 reflections with I > 2[sigma](I)

  • Rint = 0.055

Refinement
  • R[F2 > 2[sigma](F2)] = 0.042

  • wR(F2) = 0.096

  • S = 0.88

  • 12050 reflections

  • 398 parameters

  • 88 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 1.33 e Å-3

  • [Delta][rho]min = -0.89 e Å-3

Table 1
Selected bond lengths (Å)

Sb1-Br1 2.6036 (6)
Sb1-Br2 2.6292 (6)
Sb1-Br3 2.6925 (6)
Sb1-Br4 3.1222 (6)
Sb1-Br5 3.0287 (6)
Sb1-Br6 2.9558 (7)
Sb2-Br4 3.1333 (7)
Sb2-Br5 3.1602 (7)
Sb2-Br6 3.2393 (7)
Sb2-Br7 2.6068 (7)
Sb2-Br8 2.5696 (7)
Sb2-Br9 2.5713 (8)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N1-H1...Br4 0.91 2.47 3.362 (5) 168
N2A-H2A...Br3 0.91 2.43 3.23 (3) 146
N2B-H2B...Br3 0.91 2.55 3.43 (4) 162
N3A-H3A...Br6 0.91 2.4 3.25 (2) 155
N3B-H3B...Br6 0.91 2.68 3.48 (3) 148

Data collection: CrysAlis CCD (Oxford Diffraction, 2009[Oxford Diffraction (2009). CrystAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, Oxfordshire, England.]); cell refinement: CrysAlis RED (Oxford Diffraction, 2009[Oxford Diffraction (2009). CrystAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, Oxfordshire, 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: DIAMOND (Brandenburg & Berndt, 1999[Brandenburg, K. & Berndt, M. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.]) 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: VN2071 ).


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]
Brandenburg, K. & Berndt, M. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Bujak, M. & Angel, R. J. (2005). J. Solid State Chem. 178, 2237-2246.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Chaabouni, S. & Kamoun, S. (1998). Phase Transitions, 66, 119-127.  [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]
Oxford Diffraction (2009). CrystAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, Oxfordshire, 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, m353  [ doi:10.1107/S1600536813014335 ]

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