Neutral ethylene glycol (EG) molecules have been intercalated into zinc hydroxide layers to produce a new hybrid material in which only one kind of metal ion is included. Initially, layered basic zinc acetate (LBZA, Zn(5)(OH)(8)(CH(3)COO)(2).2H(2)O) was prepared from a methanolic zinc acetate dihydrate solution. The immersion of LBZA in EG resulted in its intercalation, which was accompanied by an interlayer expansion of 7.12 A, as revealed by X-ray diffractometry. A Fourier transform infrared spectroscopic study indicated that the new compound contained both the acetate groups and the EG molecules. Together with thermogravimetry-differential thermal analysis, a composition of the new compound was estimated to be Zn(5)(OH)(8)(CH(3)COO)(2)(HOC(2)H(4)OH)(2).2H(2)O. The EG intercalation was found to increase the dehydration temperature of the zinc hydroxide layers from 130 to 180 degrees C. So the thermally stable material is then promising as a new class of precursors in creating organic-inorganic nanocomposites.