Substituted alkylammonium ions ( protonated hydroxy amine and diamine) were intercalated into layered niobate K4Nb6O17 in order to introduce functional substituents into the interlayer spaces of the niobate. In the case of reaction with 3-hydroxypropylammonium ion, the intercalation compound incorporated the ammonium ions in a bilayer arrangement, by which the hydroxyl substituents were located in the middle of the interlayer spaces to form intermolecular hydrogen bonding. For the intercalation compounds with alkyldiammonium ions, the intercalated alkyldiammonium ions were present in monolayer and oriented transversally with respect to the niobate layers. (C) 2003 Kluwer Academic Publishers.