HIGH-RESOLUTION SOLID-STATE MAGIC-ANGLE-SPINNING NUCLEAR-MAGNETIC-RESONANCE STUDIES ON THE LAYERED ANTIMONY HYDROGEN PHOSPHATE, HSB(PO4)(2)CENTER-DOT-2H(2)O AND SOME ORGANIC AMINE INTERCALATION COMPOUNDS

n-propylamine and tri-n-octylamine were intercalated into the layered host antimony hydrogen phosphate, HSb(PO4)(2) . 2H(2)O (henceforth wri tten as H1SbP2). Powder X-ray diffraction (PXRD) indicated that the re action products were all polyphasic microcrystalline materials and sug gested that the arrangement of amine molecules in (i) the n-propylamin e intercalation product were similar to that observed for amine interc alated alpha-Zr(HPO4)(2) and alpha-tin (IV) hydrogen phosphates, and t hat (ii) the tri-n-octylamine molecules formed a bilayered structure w ithin the H1SbP2 interlayer in which the terminal methyl groups repuls e one another. Fourier transformed infrared (FTIR) studies also sugges ted the presence of intercalated amine molecules within the H1SbP2 lay ered 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 inter lamellar region as expected. P-31 solid-state MAS NMR studies confirme d 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 previousl y been observed for iron complexes intercalated into the H1SbP2 host.