Intercalation of ethylene glycol into layered yttrium hydroxide containing nitrate counterions was accomplished by heating the reagents in a methanol solution of sodium methoxide under autogenous pressure at 413 K for 20 h. The resulting crystalline material had an expanded interlayer distance of 10.96 angstrom, confirming the intercalation of an ethylene glycol derived species. Characterization of the material by FT-IR spectroscopy, thermogravimetric analysis, and the catalytic transesterification of tributyrin with methanol was consistent with direct bonding of ethylene glycolate anions (O2C2H5-) to the yttrium hydroxide layers, forming Y-O-C bonds. The layers of the material are proposed to be held together by H-bonding between the hydroxyls of grafted ethylene glycol molecules attached to adjacent layers. Glycerol can also be intercalated into yttrium hydroxide layered materials by a similar method.