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Volume 68 
Part 11 
Page m1392  
November 2012  

Received 10 October 2012
Accepted 11 October 2012
Online 20 October 2012

Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.003 Å
R = 0.026
wR = 0.060
Data-to-parameter ratio = 22.9
Details
Open access

(Acetylacetonato-[kappa]2O,O')dichloridobis(methanolato-[kappa]O)niobium(V)

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

In the title compound, [Nb(CH3O)2(C5H7O2)Cl2], a slightly distorted octahedral coordination geometry is observed around the NbV atom with Nb-O distances in the range of 1.8254 (16)-2.0892 (16) Å and Nb-Cl distances of 2.3997 (14) and 2.4023 (12) Å. The O-Nb-O angles vary between 81.36 (7) and 172.65 (7) °, while the trans Cl-Nb-Cl angle is 167.34 (2)°. There are no hydrogen bonds observed.

Related literature

For synthetic background, see: Herbst et al. (2010[Herbst, L., Koen, R., Roodt, A. & Visser, H. G. (2010). Acta Cryst. E66, m801-m802.]; 2011[Herbst, L., Visser, H. G., Roodt, A. & Muller, T. J. (2011). Acta Cryst. E67, m1669-m1670.]); Davies et al. (1999[Davies, H. O., Leedham, T. J., Jones, A. C., O'Brien, P., White, A. J. P. & Williams, D. J. (1999). Polyhedron, 18, 3165-3172.]). For applications of acetylacetone-type ligands in industry, see: Steyn et al. (1992[Steyn, G. J. J., Roodt, A. & Leipoldt, J. G. (1992). Inorg. Chem. 31, 3477-3481.], 1997[Steyn, G. J. J., Roodt, A., Poletaeva, I. A. & Varshavsky, Y. S. (1997). J. Organomet. Chem. 536-537, 197-205.], 2008[Steyn, M., Roodt, A. & Steyl, G. (2008). Acta Cryst. E64, m827.]); Otto et al. (1998[Otto, S., Roodt, A., Swarts, J. C. & Erasmus, J. C. (1998). Polyhedron, 17, 2447-2453.]); Roodt & Steyn (2000[Roodt, A. & Steyn, G. J. J. (2000). Recent Research Developments in Inorganic Chemistry. Vol. 2, pp. 1-23. Trivandrum, India: Transworld Research Network.]); Brink et al. (2010[Brink, A., Visser, H. G., Steyl, G. & Roodt, A. (2010). Dalton Trans. 39, 5572-5578.]); Viljoen et al. (2008[Viljoen, J. A., Muller, A. & Roodt, A. (2008). Acta Cryst. E64, m838-m839.], 2009a[Viljoen, J. A., Visser, H. G., Roodt, A. & Steyn, M. (2009a). Acta Cryst. E65, m1514-m1515.],b[Viljoen, J. A., Visser, H. G., Roodt, A. & Steyn, M. (2009b). Acta Cryst. E65, m1367-m1368.], 2010[Viljoen, J. A., Visser, H. G. & Roodt, A. (2010). Acta Cryst. E66, m603-m604.]). For related niobium complexes, see: Sokolov et al. (1999[Sokolov, M., Imoto, H., Saito, T. & Fedorov, V. (1999). J. Chem. Soc. Dalton Trans. pp. 85-92.], 2005[Sokolov, M., Gushchin, A. L., Tkachev, S. V., Naumov, D. Yu., Nunez, P., Gili, P., Platas, J. G. & Fedin, V. P. (2005). Inorg. Chim. Acta, 358, 2371-2376.]); Antinolo et al. (2000[Antinolo, A., Carrillo-Hermosilla, F., Fernandez-Baeza, J., Otero, A., Palomares, E., Rodriguez, A. M. & Sanchez-Barba, L. F. (2000). J. Organomet. Chem. 603, 194-198.]); Dahan et al. (1976[Dahan, F., Kergoat, R., Senechal-Tocquer, M. C. & Guerchais, J. E. (1976). J. Chem. Soc. Dalton Trans. pp. 2202-2209.]).

[Scheme 1]

Experimental

Crystal data
  • [Nb(CH3O)2(C5H7O2)Cl2]

  • Mr = 324.98

  • Monoclinic, P 21 /c

  • a = 7.7985 (2) Å

  • b = 11.6028 (3) Å

  • c = 14.6819 (2) Å

  • [beta] = 111.279 (1)°

  • V = 1237.91 (5) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 1.39 mm-1

  • T = 100 K

  • 0.38 × 0.13 × 0.08 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2004[Bruker (2004). SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.810, Tmax = 0.895

  • 25521 measured reflections

  • 2995 independent reflections

  • 2873 reflections with I > 2[sigma](I)

  • Rint = 0.024

Refinement
  • R[F2 > 2[sigma](F2)] = 0.026

  • wR(F2) = 0.060

  • S = 1.04

  • 2995 reflections

  • 131 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 1.90 e Å-3

  • [Delta][rho]min = -1.14 e Å-3

Data collection: APEX2 (Bruker, 2005[Bruker (2005). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2004[Bruker (2004). SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus; program(s) used to solve structure: SIR92 (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: DIAMOND (Brandenburg & Putz, 2004[Brandenburg, K. & Putz, H. (2004). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: WinGX (Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BT6846 ).


Acknowledgements

Financial assistance from the Advanced Metals Initiative (AMI) of the Department of Science and Technology (DST) of South Africa, through the New Metals Development Network (NMDN) coordinated by the South African Nuclear Energy Corporation Limited (Necsa) and the University of the Free State is gratefully acknowledged.

References

Antinolo, A., Carrillo-Hermosilla, F., Fernandez-Baeza, J., Otero, A., Palomares, E., Rodriguez, A. M. & Sanchez-Barba, L. F. (2000). J. Organomet. Chem. 603, 194-198.  [CSD] [CrossRef] [ChemPort]
Brandenburg, K. & Putz, H. (2004). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Brink, A., Visser, H. G., Steyl, G. & Roodt, A. (2010). Dalton Trans. 39, 5572-5578.  [CSD] [CrossRef] [ChemPort] [PubMed]
Bruker (2004). SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2005). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
Dahan, F., Kergoat, R., Senechal-Tocquer, M. C. & Guerchais, J. E. (1976). J. Chem. Soc. Dalton Trans. pp. 2202-2209.  [CrossRef]
Davies, H. O., Leedham, T. J., Jones, A. C., O'Brien, P., White, A. J. P. & Williams, D. J. (1999). Polyhedron, 18, 3165-3172.  [ISI] [CSD] [CrossRef] [ChemPort]
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.  [CrossRef] [ChemPort] [details]
Herbst, L., Koen, R., Roodt, A. & Visser, H. G. (2010). Acta Cryst. E66, m801-m802.  [CSD] [CrossRef] [details]
Herbst, L., Visser, H. G., Roodt, A. & Muller, T. J. (2011). Acta Cryst. E67, m1669-m1670.  [CSD] [CrossRef] [details]
Otto, S., Roodt, A., Swarts, J. C. & Erasmus, J. C. (1998). Polyhedron, 17, 2447-2453.  [ISI] [CrossRef] [ChemPort]
Roodt, A. & Steyn, G. J. J. (2000). Recent Research Developments in Inorganic Chemistry. Vol. 2, pp. 1-23. Trivandrum, India: Transworld Research Network.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Sokolov, M., Gushchin, A. L., Tkachev, S. V., Naumov, D. Yu., Nunez, P., Gili, P., Platas, J. G. & Fedin, V. P. (2005). Inorg. Chim. Acta, 358, 2371-2376.  [ISI] [CSD] [CrossRef] [ChemPort]
Sokolov, M., Imoto, H., Saito, T. & Fedorov, V. (1999). J. Chem. Soc. Dalton Trans. pp. 85-92.  [CSD] [CrossRef]
Steyn, G. J. J., Roodt, A. & Leipoldt, J. G. (1992). Inorg. Chem. 31, 3477-3481.  [CrossRef] [ChemPort] [ISI]
Steyn, G. J. J., Roodt, A., Poletaeva, I. A. & Varshavsky, Y. S. (1997). J. Organomet. Chem. 536-537, 197-205.  [CrossRef]
Steyn, M., Roodt, A. & Steyl, G. (2008). Acta Cryst. E64, m827.  [CSD] [CrossRef] [details]
Viljoen, J. A., Muller, A. & Roodt, A. (2008). Acta Cryst. E64, m838-m839.  [CSD] [CrossRef] [details]
Viljoen, J. A., Visser, H. G. & Roodt, A. (2010). Acta Cryst. E66, m603-m604.  [CSD] [CrossRef] [details]
Viljoen, J. A., Visser, H. G., Roodt, A. & Steyn, M. (2009a). Acta Cryst. E65, m1514-m1515.  [CSD] [CrossRef] [details]
Viljoen, J. A., Visser, H. G., Roodt, A. & Steyn, M. (2009b). Acta Cryst. E65, m1367-m1368.  [CrossRef] [details]


Acta Cryst (2012). E68, m1392  [ doi:10.1107/S1600536812042638 ]

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