Synthesis and structure of isopropyldimethylsilyl-substituted octamethyltitanocene |
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| Authors: | Lenka Lukešová Michal Horá?ek Ji?í Kubišta |
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| Institution: | a J. Heyrovský Institute of Physical Chemistry, Academy of Sciences of the Czech Republic, Dolejškova 3, 182 23 Prague 8, Czech Republic
b Department of Inorganic Chemistry, Faculty of Science, Charles University, Hlavova 2030, 128 40 Prague 2, Czech Republic |
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| Abstract: | Reduction of isopropyldimethylsilyl-substituted titanocene dichloride TiCl2(η5-C5Me4SiMe2Pri)2] (1) by excess magnesium in the presence of excess bis(trimethylsilyl)ethyne (btmse) in tetrahydrofuran at 60 °C yielded a mixture of products amongst them only the trinuclear Ti-Mg-Ti hydrido-bridged complex MgTi(μ-H)2(η5-C5Me4SiMe2Pri)]2 (3) was isolated and characterized. The precursor of titanocene, Ti(η5-C5Me4SiMe2Pri)2(η2-btmse)] (6), was obtained from the identical system which, after initial formation of TiCl(η5-C5Me4SiMe2Pri)2] (2), reacted at −18 °C overnight and then the solution was rapidly separated from the remaining magnesium. Titanocene Ti(η5-C5Me4SiMe2Pri)2] (7) was obtained by thermolysis of 6 at 75 °C in vacuum. Crystal structures of 1, 2, 3, 6, and 7 were determined. |
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| Keywords: | Titanium Titanocene Silyl substituent Isopropyldimethylsilyl Bis(trimethylsilyl)ethyne-titanocene thermolysis NMR spectra X-ray crystallography |
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