Zr(OPr
i
)
4
∙(Pr
i
OH) reacts with N-phenylsalicylideneimine in anhydrous benzene in 1 : 2 molar ratio to afford [Zr{O(C
6
H
4
)CH=NPh}
2
{OPr
i
}
2
] (
1
). Further reactions of
1
with various glycols yield heteroleptic complexes of the type [Zr{O(C
6
H
4
)CH=NPh}
2
{O-G-O}] [where-G-= (CH
2
)
2
(
2
), (CH
2
CHCH
3
) (
3
), (CH
3
CHCHCH
3
) (
4
), (CH
2
CHC
2
H
5
) (
5
), (CH
2
)
3
(
6
), (CH
2
CH
2
CHCH
3
) (
7
), and (CH
2
)
6
(
8
)]. All new derivatives have been characterized by elemental analyses, FTIR and NMR (
1
H and
13
C{
1
H}) 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 ZrO
2
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).