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The reaction of vanadyl acetoacetonate, VO(acac)
2
, with 2-hydroxybenzaldehyde hydrazone in ethanol
gave the mononuclear oxovanadium(IV) complex [VO(salh
1
)
2
](
1
). However, when the hydrazides
3-hydroxy-2-naphthoic acid hydrazide (h
2
) and 5-phenylisoxazole-3-carboxylicacidhydrazide (h
3
) were
used, the mononuclear oxoethoxovanadium(V) complexes [VO(acanh
2
)(OEt)] (
2
) and [VO(acanh
3
)(OEt)]
(
3
) were isolated, respectively. The reaction with benzene-1,4-dicarbohydrazide (h
4
) in a water–ethanol
solution gave polynuclear {[VO(
l
-EtO)
2
](
l
-acanh
4
)}
n
(
4
). The complexes were characterized by elemental
analysis, IR, UV–Vis and
51
V NMR spectra. Magnetic susceptibility measurements indicated the +5
vanadium oxidation state in
2
,
3
and
4
and +4 in
1
. X-ray single crystal diffraction studies revealed that
the vanadium(V) center has a distorted square pyramidal geometry in
2
and
3
, and a distorted octahedral
geometry in
4
, with an O
3
N coordination environment around the V(V) acceptor center. Complex
4
is a
polymeric compound with dihydrazide ligand as a linker and each two vanadium ions are connected
via two
l
-ethoxo bridges.