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

Lhoste, J.; Hemon-Ribaud, A.; Maisonneuve, V.; Jobic, S.; Bujoli-Doeuff, M.

doi:10.1107/S1600536812046892

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 (C-C) = 0.005 Å
R = 0.030
wR = 0.078
Data-to-parameter ratio = 24.0
Details

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

J. Lhoste,^a ^* A. Hemon-Ribaud,^a V. Maisonneuve,^a S. Jobic ^b and M. Bujoli-Doeuff ^b

^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-HO, N-HF and O-HF interactions.

Related literature

For background to the physical-chemical properties of hybrid compounds, see: Nakajima et al. (2000). For related structures containing discrete entities, see: Mattes & Lux (1976); Mattes et al. (1980); Chakravorti & Bera (1983); Adil et al. (2007); Aldous & Lightfoot (2012).

Experimental

Crystal data

(C₄H₁₄N₂)₂[Mo₂O₄F₆]·H₂O
M_r = 568.24
Monoclinic, P 2/c
a = 8.010 (2) Å
b = 8.788 (2) Å
c = 14.294 (4) Å
= 103.019 (12)°
V = 980.3 (4) Å³
Z = 2
Mo K radiation
= 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) T_min = 0.816, T_max = 0.960
35088 measured reflections
3240 independent reflections
2690 reflections with I > 2(I)
R_int = 0.036

Refinement

R[F² > 2(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
_max = 1.40 e Å^-3
_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-HA	D-H	HA	DA	D-HA
N1-H1DO1Wⁱⁱ	0.96 (4)	1.93 (4)	2.889 (3)	172 (3)
N1-H1EF3	0.87 (4)	1.94 (4)	2.760 (3)	158 (4)
N1-H1FF2ⁱⁱⁱ	0.88 (4)	1.80 (4)	2.679 (3)	178 (4)
N2-H2DF1^iv	0.93 (4)	1.87 (4)	2.779 (3)	167 (3)
N2-H2EF3^v	0.91 (4)	1.94 (4)	2.820 (3)	161 (3)
N2-H2FO1^vi	0.91 (4)	2.00 (4)	2.865 (3)	159 (3)
O1W-H1WF1	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); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 2012) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: enCIFer (Allen et al., 2004).

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.
Aldous, D. W. & Lightfoot, P. (2012). J. Fluorine Chem. 144, 108-113.
Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338.
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.
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.
Mattes, R. & Lux, G. (1976). Z. Anorg. Allg. Chem. 424, 173-182.
Mattes, R., Mennemann, K., Jäckel, N., Rieskamp, H. & Brockmeyer, H. J. (1980). J. Less-Common Met. 76, 199-212.
Nakajima, T., Zemava, B. & Tressaud, A. (2000). In Advanced Inorganic Fluorides. Lausanne: Elsevier.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

metal-organic compounds