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Volume 68 
Part 12 
Page m1520  
December 2012  

Received 7 November 2012
Accepted 14 November 2012
Online 24 November 2012

Key indicators
Single-crystal X-ray study
T = 296 K
Mean [sigma](C-C) = 0.005 Å
R = 0.030
wR = 0.078
Data-to-parameter ratio = 24.0
Details
Open access

Bis(butane-1,4-diammonium) di-[mu]-oxido-bis[trifluoridooxidomolybdate(V)] monohydrate

aLUNAM Université, Université du Maine, UMR 6283 CNRS, Institut des Molécules et des Matériaux du Mans, Avenue Olivier Messiaen, 72085 Le Mans Cedex 9, France, and bInstitut des Matériaux Jean Rouxel, UMR 6502 CNRS, 2 rue de la Houssinière, 44322 Nantes Cedex 3, France
Correspondence e-mail: jerome.lhoste@univ-lemans.fr

The title compound, (C4H14N2)2[Mo2O4F6]·H2O, was obtained by solvothermal reaction at 443 K for 72 h from a mixture of MoO3, HF, 1,4-diaminobutane (dab), water and ethylene glycol. The structure consists of [Mo2O4F6]4- anionic dimers containing strongly distorted MoO3F3 octahedra (with twofold symmetry), diprotonated dab cations and water molecules (twofold symmetry) in the ratio 1:2:1. The cohesion of the three-dimensional structure is ensured through N-H...O, N-H...F and O-H...F interactions.

Related literature

For background to the physical-chemical properties of hybrid compounds, see: Nakajima et al. (2000[Nakajima, T., Zemava, B. & Tressaud, A. (2000). In Advanced Inorganic Fluorides. Lausanne: Elsevier.]). For related structures containing discrete entities, see: Mattes & Lux (1976[Mattes, R. & Lux, G. (1976). Z. Anorg. Allg. Chem. 424, 173-182.]); Mattes et al. (1980[Mattes, R., Mennemann, K., Jäckel, N., Rieskamp, H. & Brockmeyer, H. J. (1980). J. Less-Common Met. 76, 199-212.]); Chakravorti & Bera (1983[Chakravorti, M. C. & Bera, A. K. (1983). Transition Met. Chem. 8, 83-86.]); Adil et al. (2007[Adil, K., Marrot, J., Leblanc, M. & Maisonneuve, V. (2007). Acta Cryst. E63, m1511-m1513.]); Aldous & Lightfoot (2012[Aldous, D. W. & Lightfoot, P. (2012). J. Fluorine Chem. 144, 108-113.]).

[Scheme 1]

Experimental

Crystal data
  • (C4H14N2)2[Mo2O4F6]·H2O

  • Mr = 568.24

  • Monoclinic, P 2/c

  • a = 8.010 (2) Å

  • b = 8.788 (2) Å

  • c = 14.294 (4) Å

  • [beta] = 103.019 (12)°

  • V = 980.3 (4) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 1.36 mm-1

  • T = 296 K

  • 0.15 × 0.13 × 0.03 mm

Data collection
  • Bruker APEXII diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2001[Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.816, Tmax = 0.960

  • 35088 measured reflections

  • 3240 independent reflections

  • 2690 reflections with I > 2[sigma](I)

  • Rint = 0.036

Refinement
  • R[F2 > 2[sigma](F2)] = 0.030

  • wR(F2) = 0.078

  • S = 1.05

  • 3240 reflections

  • 135 parameters

  • 1 restraint

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

  • [Delta][rho]max = 1.40 e Å-3

  • [Delta][rho]min = -0.65 e Å-3

Table 1
Selected bond lengths (Å)

Mo1-O1 1.9754 (18)
Mo1-O1i 1.9642 (18)
Mo1-O2 1.7058 (19)
Mo1-F1 2.0786 (17)
Mo1-F2 2.0612 (17)
Mo1-F3 2.1666 (15)
Symmetry code: (i) [-x+1, y, -z+{\script{1\over 2}}].

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N1-H1D...O1Wii 0.96 (4) 1.93 (4) 2.889 (3) 172 (3)
N1-H1E...F3 0.87 (4) 1.94 (4) 2.760 (3) 158 (4)
N1-H1F...F2iii 0.88 (4) 1.80 (4) 2.679 (3) 178 (4)
N2-H2D...F1iv 0.93 (4) 1.87 (4) 2.779 (3) 167 (3)
N2-H2E...F3v 0.91 (4) 1.94 (4) 2.820 (3) 161 (3)
N2-H2F...O1vi 0.91 (4) 2.00 (4) 2.865 (3) 159 (3)
O1W-H1W...F1 0.90 (1) 1.82 (1) 2.711 (3) 178 (4)
Symmetry codes: (ii) x+1, y, z; (iii) -x+1, -y+1, -z; (iv) x+1, y-1, z; (v) -x+1, -y, -z; (vi) [-x+1, y-1, -z+{\script{1\over 2}}].

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2 and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2007[Bruker (2007). APEX2 and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus; 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: ORTEP-3 (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]) and DIAMOND (Brandenburg, 1999[Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: enCIFer (Allen et al., 2004[Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: VN2059 ).


References

Adil, K., Marrot, J., Leblanc, M. & Maisonneuve, V. (2007). Acta Cryst. E63, m1511-m1513.  [CSD] [CrossRef] [details]
Aldous, D. W. & Lightfoot, P. (2012). J. Fluorine Chem. 144, 108-113.  [CrossRef] [ChemPort]
Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338.  [ISI] [CrossRef] [ChemPort] [details]
Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2007). APEX2 and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.
Chakravorti, M. C. & Bera, A. K. (1983). Transition Met. Chem. 8, 83-86.  [CrossRef] [ChemPort] [ISI]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Mattes, R. & Lux, G. (1976). Z. Anorg. Allg. Chem. 424, 173-182.  [CrossRef] [ChemPort]
Mattes, R., Mennemann, K., Jäckel, N., Rieskamp, H. & Brockmeyer, H. J. (1980). J. Less-Common Met. 76, 199-212.  [CrossRef] [ChemPort]
Nakajima, T., Zemava, B. & Tressaud, A. (2000). In Advanced Inorganic Fluorides. Lausanne: Elsevier.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]


Acta Cryst (2012). E68, m1520  [ doi:10.1107/S1600536812046892 ]

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