This disclosure describes the synthesis of layered double hydroxide compositions interlayered by polyoxometalate anionswith Keggin-type structures and having the formula [M1-x"Mx'''(OH)2]Ax/n-.yH2O, wherein, M'' is a divalent metal and M'''is a trivalent metal, A is an anionic polyoxometalate of negative charge n, x range between 0.12 to 0.8, and y is a positivenumber. The products exhibit well-defined XRD peaks corresponding to uniformly crystalline layered products with basalspacing values 14 .ANG..
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