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Volume 69 
Part 12 
Pages m673-m674  
December 2013  

Received 10 September 2013
Accepted 4 November 2013
Online 20 November 2013

Key indicators
Single-crystal X-ray study
T = 203 K
Mean [sigma](C-C) = 0.003 Å
Disorder in main residue
R = 0.036
wR = 0.086
Data-to-parameter ratio = 14.0
Details
Open access

[6,6'-Bis(1,1-di­methyl­eth­yl)-4,4'-dimethyl-2,2'-methyl­enediphenolato-[kappa]2O,O']di­chlorido­(9H-fluoren-9-ol-[kappa]O)titanium(IV)-fluorene-diethyl ether (1/0.5/1)

aChemistry, Institute of Natural and Mathematical Sciences, Massey University at Albany, PO Box 102904 North Shore Mail Centre, Auckland, New Zealand, and bInstitute of Fundamental Sciences - Chemistry, 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 adduct, [TiCl2(C23H30O2)(C13H10O]·0.5C13H10·C4H10O, is a monomer with a trigonal-bypyramidal coordination sphere of the TiIV atom in which the ligand O atoms of the bidentate diphenolate anion are located in both apical and equatorial positions. Chloride ligands occupy the remaining two equatorial sites of the trigonal bypyramid with the fluoren-9-ol O atom occupying the other apical site. The hy­droxy group H atom of this latter group is hydrogen bonded to an O atom of a non-coordinating diethyl ether mol­ecule. The title compound also contains a further fluorene solvent mol­ecule, which lies across a centre of symmetry and which is equally disordered over an inversion centre.

Related literature

For monomeric complexes of 4-coordinate titanium contain­ing the 2,2'-methyl­ene-bis-(4-methyl-6-tert-butyl­phen­o­lato) ligand, see: Toscano et al. (1998[Toscano, P. J., James Schermerhorn, E. J., Barren, E., Liu, S. & Zubieta, J. (1998). J. Coord. Chem. 43, 169-185.]). For two other structures with a five-coordinate metal atom containing this type of ligand, see: Okuda et al. (1995[Okuda, J., Fokken, S., Kang, H.-C. & Massa, W. (1995). Chem. Ber. 128, 221-227.]); Gielens et al. (1999[Gielens, E. E. C. G., Dijkstra, T. W., Berno, P., Meetsma, A., Hessen, B. & Teuben, J. H. (1999). J. Organomet. Chem. 591, 88-95.]).

[Scheme 1]

Experimental

Crystal data
  • [TiCl2(C23H30O2)(C13H10O)]·C4H10O·0.5C13H10

  • Mr = 796.71

  • Triclinic, [P \overline 1]

  • a = 12.710 (3) Å

  • b = 13.227 (3) Å

  • c = 14.431 (3) Å

  • [alpha] = 110.28 (3)°

  • [beta] = 109.22 (3)°

  • [gamma] = 91.72 (3)°

  • V = 2120.2 (7) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 0.37 mm-1

  • T = 203 K

  • 0.28 × 0.22 × 0.08 mm

Data collection
  • Siemens SMART diffractometer

  • Absorption correction: multi-scan (Blessing, 1995[Blessing, R. H. (1995). Acta Cryst. A51, 33-38.]) Tmin = 0.904, Tmax = 0.971

  • 18146 measured reflections

  • 7432 independent reflections

  • 6033 reflections with I > 2[sigma](I)

  • Rint = 0.025

Refinement
  • R[F2 > 2[sigma](F2)] = 0.036

  • wR(F2) = 0.086

  • S = 1.07

  • 7432 reflections

  • 531 parameters

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

  • [Delta][rho]max = 0.35 e Å-3

  • [Delta][rho]min = -0.37 e Å-3

Table 1
Selected bond lengths (Å)

Ti-O2 1.7755 (13)
Ti-O1 1.8040 (14)
Ti-O4 2.1485 (15)
Ti-Cl1 2.2778 (12)
Ti-Cl2 2.2963 (9)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O4-H4...O3 0.89 (3) 1.76 (3) 2.648 (2) 180 (3)

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: SHELXS90 (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, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]); software used to prepare material for publication: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BV2226 ).


Acknowledgements

This work was supported by the award of a Massey University Research Fund Post-Doctoral Fellowship to CS. We are grateful 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]
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.  [CrossRef] [ChemPort] [IUCr Journals]
Gielens, E. E. C. G., Dijkstra, T. W., Berno, P., Meetsma, A., Hessen, B. & Teuben, J. H. (1999). J. Organomet. Chem. 591, 88-95.  [CSD] [CrossRef] [ChemPort]
Okuda, J., Fokken, S., Kang, H.-C. & Massa, W. (1995). Chem. Ber. 128, 221-227.  [CrossRef] [ChemPort]
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.
Toscano, P. J., James Schermerhorn, E. J., Barren, E., Liu, S. & Zubieta, J. (1998). J. Coord. Chem. 43, 169-185.  [Web of Science] [CrossRef] [ChemPort]


Acta Cryst (2013). E69, m673-m674   [ doi:10.1107/S1600536813030249 ]

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