The topotactic exchange reactions of y-zirconium phosphate and y-zirconium phosphate/methylphosphonate with phosphonic acids derived from azacrown ethers of different sizes was examined. Prior intercalation of hexylamine was necessary in most cases to attain the maximum exchange level predicted by molecular modeling. Materials with imbricated or nonimbricated layers were obtained depending on crown size and exchange level. Exchange of methylphosphonates in y-zirconium phosphate/methylphosphonate was only observed when hexylamine had previously been intercalated. The exchange with the bisphosphonic acid derived from l,lO-diaza[l8]-crown-6 gave a material with an interlayer

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