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

摘要

Monomeric titanatrane i-PrOTi(OCMe2CH2)(3)N (1) and dimeric titanatranes [i-PrOTi(OCH2CH2)(n)N(CH2CMe2O)(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 (OCH2CH2)(n)N(CH2CMe2O)(3-n)(3-) (n = 0, Lig(1); n = 1, Lig(2): n = 2, Lig(3)), which vary by the number of CMe2 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 H-1 and C-13{H-1} 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.