Glycine intercalated vanadyl (VOPO4 . NH2CH2COOH) and niobyl (NbOPO4 .(NH2CH2COOH)(0.85). 0.45H(2)O) phosphates were prepared by shaking the reaction mixture at room temperature or by refluxing starting compounds respectively. The intercalates retain the layered structure of the parent phosphates with a basal spacing corresponding to a perpendicular arrangement of the glycine chains in the interlayer space. IR spectra confirm the presence of glycine molecules in the intercalates as zwitterionic species. Being similar to those observed for anhydrous VOPO4, impedance measurements of VOPO4 . NH2CH2COOH support the idea that the conductivity in this intercalate is electronic and the glycine molecules in the interlayer space do not take part in the conductively mechanism.