Abstract: A method of producing layered structures of metal hydroxides (one or more metals) free of chloride or chlorine is disclosed. A specific ratio layered structure hydroxide is obtained from mixing first and second metals (respectively in the form of hydroxide, oxyhydroxide carbonate or nitrate as to the first metal and a hydroxide or alkali metal oxide as to the second) in proportions yielding a precipitated layered structure. The precipitators metal hydroxides with any excess of metal over 1:1 forming a segregated phase. Processing involves mixing, maintaining as a suspension up to about 48 hours at temperatures above about 40.degree. C. followed by cooling to recover the precipitate.