Novel hybrid organic-inorganic HCa(2)Nb(3)O(10)x O\M (OM = MEA, Gly) derivatives are synthesized through the intercalation of monoethanolamine and glycine into the interplanar space of protonated layered HCa2Nb3O10 center dot yH(2)O niobate. The compounds are characterized using X-ray phase, thermogravimetric, and elemental analysis and(13)C NMR spectroscopy.