J. Twu et al., SYNTHESIS AND CHARACTERIZATION OF AN ORGANIC-INORGANIC HYBRID COMPOUND - [WO3(2,2'-BIPY)] (2,2'-BIPY = 2,2'-BIPYRIDINE), Journal of materials chemistry (Print), 8(10), 1998, pp. 2181-2184
The hydrothermal synthesis and characterization of an organic-inorgani
c hybrid compound [WO3(2,2'-bipy)] (2,2'-bipy = 2,2'-bipyridine) is pr
esented. This compound was characterized by various techniques includi
ng Raman and IR spectroscopy, XRD and thermogravimetric analysis. Stru
ctural analysis of the compound by Raman and IR data shows that it has
a novel tungstate structure with 2,2'-bipy coordinated to tungsten. T
he X-ray powder diffraction data of the compound are indexed to a mono
clinic cell with a = 14.313(4), b = 9.603(2), c = 7.288(2) Angstrom, b
eta = 102.07(2)degrees. The structure of [WO3(2,2'-bipy)] adopts a cha
in-like framework consisting of corner-shared distorted octahedra (WO4
N2) with 2,2'-bipy acting as a bidentate ligand whose rings fan out fr
om the chain. Upon heating, [WO3(2,2'-bipy)] retains its structural in
tegrity until 300 degrees C, followed by a gradual loss of 2,2'-bipy w
hich leads to the formation of WO3 at ca. 475 degrees C. The thermal d
ecomposition is observed to proceed through a transitional intermediat
e, [W4O12(2,2'-bipy)], the structure of which is proposed and discusse
d.