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Volume 68 
Part 5 
Pages m596-m597  
May 2012  

Received 28 March 2012
Accepted 5 April 2012
Online 18 April 2012

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Key indicators
Single-crystal X-ray study
T = 296 K
Mean [sigma](C-C) = 0.005 Å
R = 0.035
wR = 0.103
Data-to-parameter ratio = 16.6
Details
Open access

Bis{2-[(4-chlorophenyl)iminomethyl]pyrrol-1-ido-[kappa]2N,N'}bis(dimethylamido-[kappa]N)titanium(IV) toluene monosolvate

Zhou Chen,a Jian Wu,b Yahong Lia,b* and Bin Hua

aQinghai Institute of Salt Lakes, Chinese Academy of Sciences, Xining 810008, People's Republic of China, and bKey Laboratory of Organic Synthesis of Jiangsu Province, College of Chemistry, Chemical Engineering and Materials Science, Soochow University, Suzhou 215123, People's Republic of China
Correspondence e-mail: liyahong@suda.edu.cn

The mononuclear title compound, [Ti(C11H8ClN2)2(C2H6N)2]·C7H8, was synthesized by the reaction of N-(4-chlorophenyl)-2-pyrrolylcarbaldimine with Ti(C2H6N)4. The TiIV ion is situated on a twofold rotation axis and displays a distorted octahedral geometry defined by four N atoms from two 2-[(4-chlorophenyl)iminomethyl]pyrrol-1-ide ligands and two N atoms from two dimethylamine ligands. The Ti-Npyrrole bond length [2.1041 (19) Å] is longer than the Ti-Ndimethylamine bond length [1.9013 (19) Å]; the imine N atom exhibits the longest Ti-N bond [2.3152 (17) Å]. The toluene solvent molecule is located on a twofold rotation axis running through the C atom of the methyl group. Consequently, the H atoms of the latter are rotationally disordered. The compound contains no markable hydrogen-bonding interactions.

Related literature

For the synthesis of N-(4-chlorophenyl)-2-pyrrolylcarbaldimine and its oxidovanadium(IV) complexes, see: Mozaffar et al. (2010[Mozaffar, A., Mohammad Hadi, G., Susan, T., Khosro, M. & Fatemeh, M. (2010). J. Chem. Sci. 122, 539-548.]). For the synthesis of titanium amido complexes and their applications in hydroamination reactions, see: Ramanathan et al. (2004[Ramanathan, B., Keith, A. J., Armstrong, D. & Odom, A. L. (2004). Org. Lett. 6, 2957-2960.]); Cao et al. (2001[Cao, C., Ciszewski, J. T. & Odom, A. L. (2001). Organometallics, 20, 5011-5013.]); Bexrud et al. (2007[Bexrud, J. A., Li, C. & Schafer, L. L. (2007). Organometallics, 26, 6366-6372.]); Tillack et al. (2005[Tillack, A., Khedkar, V., Jiao, H. & Beller, M. (2005). Eur. J. Org. Chem. pp. 5001-5012.]); Braunschweig & Breitling (2006[Braunschweig, H. & Breitling, F. M. (2006). Coord. Chem. Rev. 250, 2691-2720.]); Zhao et al. (2012[Zhao, Y., Lin, M., Chen, Z., Pei, H., Li, Y., Chen, Y., Wang, X., Li, L., Cao, Y., Zhang, Y. & Li, W. (2012). RSC Adv. 2, 144-150.]).

[Scheme 1]

Experimental

Crystal data

  • [Ti(C11H8ClN2)2(C2H6N)2]·C7H8

  • Mr = 635.48

  • Orthorhombic, P 21 21 2

  • a = 11.1952 (4) Å

  • b = 13.8545 (6) Å

  • c = 10.4651 (3) Å

  • V = 1623.18 (10) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 0.46 mm-1

  • T = 296 K

  • 0.27 × 0.25 × 0.20 mm
Data collection

  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.886, Tmax = 0.914

  • 7377 measured reflections

  • 3172 independent reflections

  • 2855 reflections with I > 2[sigma](I)

  • Rint = 0.021
Refinement

  • R[F2 > 2[sigma](F2)] = 0.035

  • wR(F2) = 0.103

  • S = 1.04

  • 3172 reflections

  • 191 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.24 e Å-3

  • [Delta][rho]min = -0.81 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 1338 Friedel pairs

  • Flack parameter: 0.00 (3)

Data collection: APEX2 (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS 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: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2614 ).

Acknowledgements

The authors appreciate financial support from the Hundreds of Talents Program (2005012) of the CAS, the Natural Science Foundation of China (20872105), the Qinglan Project of Jiangsu Province (Bu109805) and the Open Project of the Key Laboratory for Magnetism and Magnetic Materials of the Ministry of Education of Lanzhou University (LZUMMM2010003).

References

Bexrud, J. A., Li, C. & Schafer, L. L. (2007). Organometallics, 26, 6366-6372.  [CSD] [CrossRef] [ChemPort]
Braunschweig, H. & Breitling, F. M. (2006). Coord. Chem. Rev. 250, 2691-2720.  [ISI] [CrossRef] [ChemPort]
Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Cao, C., Ciszewski, J. T. & Odom, A. L. (2001). Organometallics, 20, 5011-5013.  [CrossRef] [ChemPort]
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Mozaffar, A., Mohammad Hadi, G., Susan, T., Khosro, M. & Fatemeh, M. (2010). J. Chem. Sci. 122, 539-548.
Ramanathan, B., Keith, A. J., Armstrong, D. & Odom, A. L. (2004). Org. Lett. 6, 2957-2960.  [ISI] [CrossRef] [PubMed] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Tillack, A., Khedkar, V., Jiao, H. & Beller, M. (2005). Eur. J. Org. Chem. pp. 5001-5012.  [CrossRef]
Zhao, Y., Lin, M., Chen, Z., Pei, H., Li, Y., Chen, Y., Wang, X., Li, L., Cao, Y., Zhang, Y. & Li, W. (2012). RSC Adv. 2, 144-150.  [CSD] [CrossRef] [ChemPort]

Acta Cryst (2012). E68, m596-m597   [ doi:10.1107/S1600536812014961 ]

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