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Polytypism in sulfate-intercalated layered double hydroxides of Zn and M(III) (M = Al, Cr): observation of cation ordering in the metal hydroxide layers.

The as-precipitated sulfate-intercalated layered double hydroxide of Zn and Al crystallizes in the structure of the 3R1 polytype. On hydrothermal treatment, this 3R1 polytype transforms into the somewhat rare 3H and 3R2 polytypes at different temperatures. Observation of the 3R2 polytype distinct from the 3R1 polytype is evidence for the lack of cation ordering in the [Zn-Al-SO4] system. The layered double hydroxide of Zn and Cr (polytype, 1H) on hydrothermal treatment in mother liquor yields a cation-ordered phase also having the structure of the 1H polytype. Direct evidence of cation ordering is found by the appearance of weak supercell reflections corresponding to a = √3 × a(o) (a(o) is the a parameter of the cation-disordered phase). The same precursor under other conditions yields the cation-disordered 3R1 polytype. In this work, the structures of both the cation-ordered and the cation-disordered phases with similar states of hydration are refined and compared.