The oxovanadium(V) complex <
B>4 can
be readily synthesized
by the reaction of the lithium salt of
p-methylhexahomotrioxacalix[3]arene trianion
3 withVOCl
3. Infrared spectra indicate a terminal V=O forcomplex
4in solution and V=O···V dative interactions in the solid stateconsistent with the formation of a
-oxo-
bridgedlinear chain polymer
1 (M = V, Y = O, X
3 =trianion of macrocycle
2a). Vanadium-51 NMR spectraindicateincreased shielding for the linear chain polymer in the solid statecompared to complex
4 in solution. Complex
4 and its linear chain polymer are proposed to have theoxovanadium group contained within the cup of themacrocycle ligand as shown in structures
5 and
7,respectively, where the
cone represents macrocycle
2a.