Year 2005, Month 12 (Section Full Articles, Page 2831)
Synthesis of new titanatranes containing organic substituents
in the atrane fragment
K. V. Zaitsev (a), S. S. Karlov (a), M. V. Zabalov (a), A. V. Churakov (b), G. S. Zaitseva (a), and D. A. Lemenovskii (a)
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.
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