n-propylamine and tri-n-octylamine were intercalated into the layered host antimony hydrogen phosphate, HSb(PO4)(2) . 2H(2)O (henceforth written as H1SbP2). Powder X-ray diffraction (PXRD) indicated that the reaction products were all polyphasic microcrystalline materials and suggested that the arrangement of amine molecules in (i) the n-propylamine intercalation product were similar to that observed for amine intercalated alpha-Zr(HPO4)(2) and alpha-tin (IV) hydrogen phosphates, and that (ii) the tri-n-octylamine molecules formed a bilayered structure within the H1SbP2 interlayer in which the terminal methyl groups repulse one another. Fourier transformed infrared (FTIR) studies also suggested the presence of intercalated amine molecules within the H1SbP2 layered structure. High-resolution N-15 solid-state magic-angle spinning nuclear magnetic resonance (MAS NMR) indicated that for both reaction products a single amine species was intercalated into the H1SbP2 interlamellar region as expected. P-31 solid-state MAS NMR studies confirmed that the intercalating amine species were all protonated and that in the case of the n-propylamine reaction products, there were a variety of orientated intercalating species. P-31 MAS MMR also suggested that there was perturbation of the adjacent phosphate groups by the large tri-n-octylamine alkyl chains. This type of perturbation has previously been observed for iron complexes intercalated into the H1SbP2 host.