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Tungsten alkoxides of the WO(OR)/sub 4/ series

Journal Article · · Sov. J. Coordinat. Chem.; (United States)
OSTI ID:6413735

The compounds WO(OR)/sub 4/ (I) (where R = Me, Et, i-Pr, n-Bu) have been synthesized with quantitative yields by reacting ethereal solutions of WOCl/sub 4/ with alcoholic solutions of NaOR at 0/sup 0/C. It has been established that the method for the synthesis of I described in the literature, which involves the preliminary alcoholysis of WOCl/sub 4/, results in the contamination of I by hydrolysis products, i.e., WO/sub 2/(OR)/sub 2/. The solubility polytherm of WO(OEt)/sub 4/ in EtOH has been studied up to the melting point of the alkoxide (126/sup 0/C). It has been established mass-spectrometrically that the transition to the gaseous phase is accompanied by the disproportionation of WO(OR)/sub 4/ to W(OR)/sub 6/ and WO/sub 2/(OR)/sub 2/, whose presence was also discovered in the x-ray diffraction analysis of the sublimation products of WO(OMe)/sub 4/. The compound WO(OBu-t)/sub 4/ sublimes without decomposition. Similarity between the structures of the methoxide and the ethoxide and that of WOCl/sub 4/ (the positioning of (trans-WO/sub 2/L/sub 4/) octahedrons at the vertices and center of a tetragonal cell) has been established on the basis of x-ray powder diffraction investigations. The IR-spectroscopic data confirm the existence in structure I of O dot-dot-dot/single bond W-O bridges (the absorption bands at 800 and 600 cm/sup -1/ correspond to two types of bonds, viz, dot-dot-dot/single bond W-O dot-dot-dot/single bond W and W-OR) and mono- or oligomeric WO(OBu-t)/sub 4/ molecules (the band at 950 cm/sup -1/ corresponds to terminal W=O bonds). The diffuse reflectance spectra in the 40,000-4000-cm/sup -1/ region have been presented.

Research Organization:
M.V. Lomonosov Moscow State Univ., USSR
OSTI ID:
6413735
Journal Information:
Sov. J. Coordinat. Chem.; (United States), Journal Name: Sov. J. Coordinat. Chem.; (United States) Vol. 11:11; ISSN SJCCD
Country of Publication:
United States
Language:
English