Layered zincophosphate materials were prepared from the molecular precursor Zn4(μ4-O)[O2P(OtBu)2]6 (1) via thermolysis (180−215 °C) in anhydrous organic solvents in the presence of long-chain primary amines. Through variation of the amine concentration, two series of materials were obtained with the stoichiometries Zn2(HPO4)3(H3NCnH2n+1)2 and Zn2(HPO4)3(H3NCnH2n+1)2(H2NCnH2n+1) (n = 8−16). These materials possess an unusual Zn/P ratio of 2:3 which is uncommon for layered zincophosphate materials prepared in aqueous media.
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