129Xe NMR spectroscopy of xenon gas absorbed in clays and pillared clays has been used to glean information on the interlayer gallery height of clays before and after pillaring. Two clay minerals were study, a Ca2+ - montmorilonite and Bentonite L. The NMR results indicate that the effective interlamellar spacing of the montmorillonite increased from 5.4 to 8.0A after pillaring with aluminum polyoxohydroxy cations. These data are consistent with X-ray powder diffraction results, which show a corresponding increase in gallery height from 5.6 to 8.4A.