Vanadate complexes bearing an imidazolidine-bridged bis(aryloxido) ligand: synthesis and solid state and solution structureCCDC 855050 for H2L. For crystallographic data in CIF or other electronic format see 10.1039/c2dt30153a
A new imidazolidine-bridged bis(aryloxido) ligand precursor ( H 2 L ) [ H 2 L = 2,2-(imidazolidine-1,3-diylbis(methylene))bis(4-(1,1,3,3-tetramethylbutyl-2-yl)phenol)] was prepared in a relatively high yield (60%) via a single-step Mannich condensation of 4-(1,1,3,3-tetramethylbutyl)phenol, ethylene...
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Zusammenfassung: | A new imidazolidine-bridged bis(aryloxido) ligand precursor (
H
2
L
) [
H
2
L
= 2,2-(imidazolidine-1,3-diylbis(methylene))bis(4-(1,1,3,3-tetramethylbutyl-2-yl)phenol)] was prepared in a relatively high yield (60%)
via
a single-step Mannich condensation of 4-(1,1,3,3-tetramethylbutyl)phenol, ethylenediamine and paraformaldehyde at 2:1:3 molar ratio and characterized by chemical and physical techniques including X-ray crystallography. Reactions of
H
2
L
with [VO(OEt)
3
] at 1:1 and 1:2 molar ratios in toluene afforded [V(L-
3
O,N,N,O)(O)(OEt)] (
1
) and [V
2
(-L-
4
O,N,N,O)(-OEt)
2
(O)
2
(OEt)
2
] (
2
), respectively. Alcoholysis of
1
with EtOH enables elimination of one molecule of
H
2
L
and the formation of
2
. Compounds
1
and
2
were characterized by IR and NMR spectroscopy as well as ES-MS experiments. The definitive molecular structure of
2
was provided by a single-crystal analysis and revealed its dinuclear nature, featuring two octahedral vanadium centres bridged by both OEt groups and the L ligand. The
51
V,
1
H and
13
C NMR spectra as well as ES-MS showed that
2
does not stay intact in solution and undergoes dissociation to give
1
and [VO(OEt)
3
].
The synthesis, structure and spectroscopic characteristics of the 2,2-(imidazolidine-1,3-diylbis(methylene))bis(4-(1,1,3,3-tetramethylbutyl-2-yl)phenol and its corresponding vanadate complexes are reported. |
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ISSN: | 1477-9226 1477-9234 |
DOI: | 10.1039/c2dt30153a |