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Volume 69 
Part 12 
Pages m676-m677  
December 2013  

Received 7 November 2013
Accepted 19 November 2013
Online 23 November 2013

Key indicators
Single-crystal X-ray study
T = 150 K
Mean [sigma](C-C) = 0.002 Å
R = 0.022
wR = 0.061
Data-to-parameter ratio = 17.5
Details
Open access

Bis([mu]-2-hy­droxy­methyl-2-methyl­propane-1,3-diolato)bis­[di­chlorido­titanium(IV)] diethyl ether disolvate

aChemistry, Institute of Natural and Mathematical Sciences, Massey University at Albany, PO Box 102904 North Shore Mail Centre, Auckland, New Zealand, and bChemistry, Institute of Fundamental Sciences, Massey University at Albany, PO Box 102904 North, Shore Mail Centre, Auckland, New Zealand
Correspondence e-mail: a.j.nielson@massey.ac.nz

The title complex, [Ti2Cl4{CH3C(CH2O)2(CH2OH)}2], lies across a centre of symmetry with a diethyl ether solvent mol­ecule hydrogen bonded to the -CH2OH groups on either side of it. The TiIV atom is coordinated in a distorted octa­hedral geometry by a tripodal ligand and two terminal chloride atoms. There are three coordination modes for the tripodal ligand distinguishable on the basis of their very different Ti-O bond lengths. For the terminal alkoxo ligand, the Ti-O distance is 1.760 (1) Å, the asymmetric bridge system has Ti-O bond lengths of 1.911 (1) and 2.048 (1) Å. The Ti-O bond length for the alcohol O atom is the longest at 2.148 (1) Å.

Related literature

For general background to Ti-O and Ti-Cl bonds, see: Gau et al. (1996[Gau, H.-M., Lee, C.-S., Lin, C.-C. & Jiang, M.-K. (1996). J. Am. Chem. Soc. 118, 2936-2941.]); Wu et al. (1996[Wu, Y.-T., Ho, Y.-C., Lin, C.-C. & Gau, H.-M. (1996). Inorg. Chem. 35, 5948-5952.]). For closely related structures, see: Talbot-Eeckelaers et al. (2006[Talbot-Eeckelaers, C. E., Rajaraman, G., Cano, J., Aromí, G., Ruiz, E. & Brechin, E. K. (2006). Eur. J. Inorg. Chem. pp. 3382-3392.]); Chang et al. (1993[Chang, Y., Chen, Q., Khan, M. I., Salta, J. & Zubieta, J. (1993). J . Chem. Soc. Chem. Commun. pp. 1872-1874.]); Salta & Zubieta (1997[Salta, J. & Zubieta, J. (1997). Inorg. Chim. Acta, 257, 83-88.]); Chen et al. (1997[Chen, Q., Chang, Y. D. & Zubieta, J. (1997). Inorg, Chim. Acta, 258, 257-262.]). For cluster compounds of this ligand type, see: Boyle et al. (1995[Boyle, T. J., Schwartz, R. W., Doedens, R. J. & Ziller, J. W. (1995). Inorg. Chem. 34, 1110-1120.]); Delmont et al. (2000[Delmont, R., Proust, A., Robert, F., Herson, P. & Gourzerh, P. (2000). Chimie, 3, 147-155.]); Liu et al. (1990[Liu, S., Ma, L., McGowty, D. & Zubieta, J. (1990). Polyhedron, 9, 1541-1553.]).

[Scheme 1]

Experimental

Crystal data
  • [Ti2Cl4(C5H10O3)2]·2C4H10O

  • Mr = 622.10

  • Triclinic, [P \overline 1]

  • a = 7.9617 (3) Å

  • b = 9.6379 (4) Å

  • c = 10.5783 (5) Å

  • [alpha] = 71.351 (1)°

  • [beta] = 82.023 (1)°

  • [gamma] = 66.757 (1)°

  • V = 706.60 (5) Å3

  • Z = 1

  • Mo K[alpha] radiation

  • [mu] = 0.98 mm-1

  • T = 150 K

  • 0.26 × 0.24 × 0.10 mm

Data collection
  • Siemens SMART CCD diffractometer

  • Absorption correction: multi-scan (Blessing, 1995[Blessing, R. H. (1995). Acta Cryst. A51, 33-38.]) Tmin = 0.766, Tmax = 0.892

  • 6510 measured reflections

  • 2661 independent reflections

  • 2417 reflections with I > 2[sigma](I)

  • Rint = 0.015

Refinement
  • R[F2 > 2[sigma](F2)] = 0.022

  • wR(F2) = 0.061

  • S = 1.04

  • 2661 reflections

  • 152 parameters

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

  • [Delta][rho]max = 0.31 e Å-3

  • [Delta][rho]min = -0.27 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O3-H3...O11 0.74 (2) 1.89 (2) 2.6233 (14) 168 (2)

Data collection: SMART (Siemens, 1995[Siemens (1995). SAINT and SMART. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Siemens, 1995[Siemens (1995). SAINT and SMART. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; 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 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]); software used to prepare material for publication: SHELXL97.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HG5360 ).


Acknowledgements

We are grateful to Massey University for the award of a Post-Doctoral Fellowship to CS, and to Ms T. Groutso of the University of Auckland for the data collection.

References

Blessing, R. H. (1995). Acta Cryst. A51, 33-38.  [CrossRef] [IUCr Journals]
Boyle, T. J., Schwartz, R. W., Doedens, R. J. & Ziller, J. W. (1995). Inorg. Chem. 34, 1110-1120.  [CSD] [CrossRef] [ChemPort] [Web of Science]
Chang, Y., Chen, Q., Khan, M. I., Salta, J. & Zubieta, J. (1993). J . Chem. Soc. Chem. Commun. pp. 1872-1874.  [CrossRef] [Web of Science]
Chen, Q., Chang, Y. D. & Zubieta, J. (1997). Inorg, Chim. Acta, 258, 257-262.
Delmont, R., Proust, A., Robert, F., Herson, P. & Gourzerh, P. (2000). Chimie, 3, 147-155.  [ChemPort]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Gau, H.-M., Lee, C.-S., Lin, C.-C. & Jiang, M.-K. (1996). J. Am. Chem. Soc. 118, 2936-2941.  [CSD] [CrossRef] [ChemPort] [Web of Science]
Liu, S., Ma, L., McGowty, D. & Zubieta, J. (1990). Polyhedron, 9, 1541-1553.  [CSD] [CrossRef] [ChemPort] [Web of Science]
Salta, J. & Zubieta, J. (1997). Inorg. Chim. Acta, 257, 83-88.  [CSD] [CrossRef] [ChemPort] [Web of Science]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Siemens (1995). SAINT and SMART. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.
Talbot-Eeckelaers, C. E., Rajaraman, G., Cano, J., Aromí, G., Ruiz, E. & Brechin, E. K. (2006). Eur. J. Inorg. Chem. pp. 3382-3392.
Wu, Y.-T., Ho, Y.-C., Lin, C.-C. & Gau, H.-M. (1996). Inorg. Chem. 35, 5948-5952.  [CSD] [CrossRef] [ChemPort] [Web of Science]


Acta Cryst (2013). E69, m676-m677   [ doi:10.1107/S1600536813031504 ]

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