Keywords:Intercalations / Powder X-ray diffraction / Vibrational spectroscopy / ab initio calculations Intercalation compounds of vanadyl phosphate and isostructural niobyl arsenate with γ-butyrolactone, VOPO 4 ·C 4 H 6 O 2 and NbOAsO 4 ·C 4 H 6 O 2 , respectively, were prepared from corresponding propanol intercalates by molecular exchange in a microwave field. The prepared intercalates were characterized using powder X-ray diffraction, density measurements, and thermogravimetric analysis. Infrared and Raman spectra indicate a coordination of the carbonyl oxygen atom of the γ-butyrolactone molecule to the vanadium or niobium