Synthesis of new titanatranes containing organic substituents in the atrane fragment |
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| Authors: | K V Zaitsev S S Karlov M V Zabalov A V Churakov G S Zaitseva D A Lemenovskii |
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| Institution: | (1) Department of Chemistry, M. V. Lomonosov Moscow State University, 1 Leninskie Gory, 119992 Moscow, Russian Federation;(2) N. S. Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences, 31 Leninsky prosp., 119991 Moscow, Russian Federation |
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| Abstract: | Titanatrane CpTi(OCH(CH3)CH2)3N (3) was prepared by the reaction of CpTiCl3 with N(CH2CH(CH3)OH)3 in the presence of triethylamine. The reaction of CpTi(OMe)3 (8) with N(CH2CH2OH)2(CH2CHPhOH), erythro-N(CH2CH2OH)2(CHPhCHPhOH), and N(CH2CH2OH)2(CH2CPh2OH) gave cyclopentadienyltitanatranes 12–14. Compound 8 reacts with threo-N(CH2CH2OH)2(CHPhCHPhOH) to give a mixture of threo-CpTi(OCH2CH2)2(OCHPhCHPh)N and threo-MeOTi(OCH2CH2)2(OCHPhCHPh)N. Slow hydrolysis of the latter product gave threo-Ti3O(OMe){(OCH2CH2)2− (OCHPhCHPh)N} 3]2, which was studied by X-ray diffraction analysis. The crystal structures of 3 and 12 were also determined by X-ray diffraction analysis. The titanium coordination polyhedron in these complexes is a distorted
trigonal bipyramid in which the equatorial positions are occupied by three oxygen atoms and the axial positions contain the
N atom and the Cp group. The titanium—nitrogen distances (2.313(2), 2.291(2) Å in two independent molecules of 3 and 2.271(2) Å in compound 12) confirm the presence of Ti←N transannular interaction.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2736–2744, December, 2005. |
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| Keywords: | titanatranes trialkanolamines transalkoxylation transannular interaction X-ray diffraction analysis |
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