trans-Bis(1,3-diphenyl­propane-1,3-dionato)(methanol)oxidovanadium(IV) methanol disolvate

Pretorius, C.; Venter, J.A.; Roodt, A.

doi:10.1107/S1600536812044686

Volume 68
Part 12
Pages m1442-m1443
December 2012

Received 25 September 2012
Accepted 29 October 2012
Online 3 October 2012

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.003 Å
R = 0.041
wR = 0.102
Data-to-parameter ratio = 17.8
Details

trans-Bis(1,3-diphenylpropane-1,3-dionato)(methanol)oxidovanadium(IV) methanol disolvate

Carla Pretorius,^a ^* Johan A. Venter ^a and Andreas Roodt ^a

^aDepartment of Chemistry, University of the Free State, PO Box 339, Bloemfontein 9300, South Africa
Correspondence e-mail: CPretorius@ufs.ac.za

In the title compound, [V(C₁₅H₁₁O₂)₂O(CH₃OH)]·2CH₃OH, the V^IV atom is coordinated by two 1,3-diphenylpropane-1,3-dionate ligands and an oxide ligand in an axial position. The sixth position is occupied by the O atom of a methanol group bonded trans to the oxide atom. The octahedral geometry is significantly distorted, with the V^IV atom lying 0.330 (3) Å above the equatorial plane formed by the O atoms of the two [beta] -diketonate ligands. In the crystal, O-HO hydrogen bonds between the coordinating methanol group in the complex and the two methanol solvent molecules lead to the formation of polymeric chains along the c-axis direction. Weak C-HO contacts are also observed.

Related literature

For synthetic background, see: Schilde et al. (1995). For other methanol-substituted vanadium complexes, see: Gao et al. (1998); Chen et al. (2004); Tasiopoulos et al. (1999). For methoxy-substituted vanadium complexes, see: Bansse et al. (1992).

Experimental

Crystal data

[V(C₁₅H₁₁O₂)₂O(CH₄O)]·2CH₄O
M_r = 609.54
Monoclinic, P 2₁ /c
a = 16.1411 (1) Å
b = 10.7450 (6) Å
c = 18.5378 (13) Å
= 113.579 (2)°
V = 2946.7 (3) Å³
Z = 4
Mo K radiation
= 0.39 mm^-1
T = 100 K
0.47 × 0.07 × 0.05 mm

Data collection

Bruker APEXII KappaCCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2008) T_min = 0.968, T_max = 0.981
38614 measured reflections
7317 independent reflections
5545 reflections with I > 2(I)
R_int = 0.046

Refinement

R[F² > 2(F²)] = 0.041
wR(F²) = 0.102
S = 1.03
7317 reflections
412 parameters
H atoms treated by a mixture of independent and constrained refinement
_max = 0.45 e Å^-3
_min = -0.43 e Å^-3

Table 1
Selected bond lengths (Å)

O1-V1	1.5965 (13)
O2-V1	1.9972 (12)
O3-V1	2.0045 (12)
O4-V1	1.9847 (12)
O5-V1	1.9935 (12)
O6-V1	2.3020 (15)

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O6-H6AO7	0.82 (3)	1.83 (3)	2.644 (2)	169 (3)
O7-H7AO8ⁱ	0.87 (3)	1.90 (3)	2.749 (2)	168 (3)
O8-H8AO3	0.90 (3)	1.96 (3)	2.853 (2)	178 (3)
C13-H13O1ⁱⁱ	0.95	2.58	3.487 (2)	160
C32-H32BO1ⁱ	0.98 (3)	2.43 (3)	3.360 (3)	159 (2)
Symmetry codes: (i) $[x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (ii) $[-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

Data collection: APEX2 (Bruker, 2011); cell refinement: SAINT-Plus (Bruker, 2008); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: Mercury (Macrae et al., 2008); software used to prepare material for publication: WinGX (Farrugia, 1999), publCIF (Westrip, 2010), PARST (Nardelli, 1995) and PLATON (Spek, 2009).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SJ5267 ).

Acknowledgements

Financial assistance from the University of the Free State Strategic Academic Cluster Initiative (Materials and Nanosciences), SASOL and the South African National Research Foundation (SA-NRF/THRIP) is gratefully acknowledged.

References

Bansse, W., Ludwig, E., Uhlemann, E., Weller, F., Dehnicke, K. & Herrmann, W. (1992). Z. Anorg. Allg. Chem. 613, 36-44.
Bruker (2008). SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2011). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
Chen, C. T., Lin, J. S., Kuo, J. H., Weng, S. S., Cuo, T. S., Lin, Y. W., Cheng, C. C., Huang, Y. C., Yu, J. K. & Chou, P. T. (2004). Org. Lett. 6, 4471-4474.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
Gao, S., Weng, Z. & Liu, S. (1998). Polyhedron, 17, 3595-3606.
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.
Nardelli, M. (1995). J. Appl. Cryst. 28, 659.
Schilde, U., Bannse, W., Ludwig, E. & Uhlemann, E. (1995). Z. Kristallogr. 210, 627-628.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148-155.
Tasiopoulos, A. J., Troganis, A. N., Evangelou, A., Raptopoulou, C. P., Terzis, A., Deligiannakis, Y. & Kabanos, T. A. (1999). Chem. Eur. J. 5, 910-921.
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.

metal-organic compounds