Selective synthesis of monomeric or dimeric titanatranes via fine tuning in triethanolateamine ligand

Abstract

Monomeric titanatrane i-PrOTi(OCMe(2)CH(2))(3)N (1) and dimeric titanatranes [i-PrOTi(OCH(2)CH(2))(n)N(CH(2)CMe(2)O)(3-n)](2) (n = 1, 2; n = 2, 3) were synthesized by the reaction of Ti(O-i-Pr)(4) with a series of triethanolateamines such as (OCH(2)CH(2))(n)N(CH(2)CMe(2)O)(3-n)(3-) (n = 0, Lig(1); n = 1, Lig(2): n = 2, Lig(3)), which vary by the number of CMe(2) groups adjacent to a CH functionality from 3 (Lig(1)H(3)) to 2 (Lig(2)H(3)) to 1 (Lig(3)H(3)). The resultant titanatranes 1-3 have been characterized by Solution (1)H and (13)C{(1)H} NMR and their solid state structures have been determined by X-ray crystallography. Whereas compound 1 is monomeric in the solid state, compounds 2 and 3 are dimeric, due to the reduction of the steric congestion in the vicinity of the Ti. (C) 2009 Elsevier Ltd. All rights reserved.