| Abstract: | Zr(OPri)4·PriOH reacts with N-phenylsalicylideneimine in anhydrous benzene in 1 : 2 molar ratio to afford Zr{O(C6H4)CH=NPh}2{OPri}2] (1). Further reactions of 1 with various glycols yield heteroleptic complexes of the type Zr{O(C6H4)CH=NPh}2{O–G–O}] where–G–= (CH2)2 (2), (CH2CHCH3) (3), (CH3CHCHCH3) (4), (CH2CHC2H5) (5), (CH2)3 (6), (CH2CH2CHCH3) (7), and (CH2)6 (8)]. All new derivatives have been characterized by elemental analyses, FTIR and NMR (1H and 13C{1H}) studies. FAB mass spectra of 1 and 7 revealed the monomeric nature of these complexes. Complete hydrolyses and low temperature transformations of 1 and 7 using Sol-Gel technique formed tetragonal phase of ZrO2 at 700°C, whereas transformation of tetragonal to monoclinic phase occurred at 900°C. SEM observations of these samples indicate formation of agglomerates of nanocrystalline zirconia (Scherer analysis). |
