Research Article: Trichlorido{2-[2-(η5-cyclo­penta­dien­yl)-2-methyl­prop­yl]-1-trimethyl­silyl-1H-imidazole-κN3}titanium(IV) tetra­hydro­furan hemisolvate

Date Published: May 01, 2010

Publisher: International Union of Crystallography

Author(s): Fang Ge, Wanli Nie, Maxim V. Borzov, Andrei V. Churakov.


The title compound, [Ti(C15H23N2Si)Cl3]·0.5C4H8O, has been prepared from {2-[2-(η5-cyclo­penta­dien­yl)-2-methyl­prop­yl]-1H-imidazolyl-κN1}bis­(N,N-diethyl­amido-κN)titanium(IV), (C12H14N2)Ti(NEt2)2, by reaction with excess of Me3SiCl in tetra­hydro­furan (THF) at 353 K. The crystal structure contains THF as adduct solvent, disordered around a center of inversion. The presence of THF and the adduct ratio has been independently supported by 1H NMR spectroscopy. The coordination polyhedron of the Ti atom is distorted square-pyramidal, assuming the cyclo­penta­dienyl (Cp) ring occupies one coordination site. The Ti, Si and CH2 group C atoms only deviate slightly from the imidazole ring plane [by 0.021 (4), 0.133 (4) and 0.094 (4) Å, respectively]. Comparison of the principal geometric parameters with those of the few known structurally characterized analogues reveal small differences in bond lengths and angles at the Ti atom. The title complex is only stable in THF-d8 in the presence of excess Me3SiCl, otherwise it exists in an equilibrium with equimolar amounts of dichlorido{2-[2-(η5-cyclo­penta­dien­yl)-2-methyl­prop­yl]-1H-imidazolyl-κN3}titanium(IV) and chloro­trimethyl­silane.

Partial Text

For a description of cyclo­penta­dienes with pendant 1H-imidazol(in)-2-yl side-chain functional groups and group 4 transition metal complexes of general type [η5-Cp-(CPh2CH2)-imidazol(in)e)-κN3]-MIVCl3 (M = Ti, Zr) , see: Krut’ko et al. (2006 ▶); Nie et al. (2008 ▶). For the geometric parameters of structurally characterized TiIV complexes of the similar η5-CpTiCl3-NRn type, see: trichloro­{2-[2-(η5-cyclo­penta­dien­yl)-2,2-diphenyl­ethyl]-1-methyl-1H-imidazole-κN3}titanium(IV), C23H21Cl3N2Ti (Krut’ko et al., 2006 ▶); trichloro­{1-[2-(η5-cyclo­penta­dien­yl)eth­yl]pyrrolidine-κN}titanium(IV), C11H16Cl3NTi (Herrmann et al., 1995 ▶); trichloro­[8-(η5-2,3,4,5-tetra­methyl­cyclo­penta­dien­yl)quinoline-κN]titanium(IV), C18H18Cl3NTi (Enders et al., 1997 ▶); trichloro­[8-(η5-2,3-dimethyl­cyclo­penta­dien­yl)quinoline-κN]titanium(IV), C16H14Cl3NTi (Enders et al., 1996 ▶). For the preparation of [2-[2-(η5-cyclo­penta­dien­yl)-2-methyl­prop­yl]-1H-imidazolyl-κN1]bis­(N,N-di­ethyl­amido-κN)titanium(IV), (C12H14N2)Ti(NEt2)2, see: Wang et al. (2009 ▶). For a description of the Cambridge Structural Database, see: Allen (2002 ▶).




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