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High\u2010quality <jats:sup>17<\/jats:sup>O solid\u2010state NMR spectra are obtained, for the first time, for LDHs prepared with only several hundred microliters of <jats:sup>17<\/jats:sup>O\u2010enriched H<jats:sub>2<\/jats:sub>O. The <jats:sup>17<\/jats:sup>O resonances due to the different oxygen ions in the structure of LDHs can be resolved with better resolution than the results obtained from <jats:sup>1<\/jats:sup>H ultrafast magic angle spinning (MAS) NMR spectroscopy. The results show clear evidence for Al\u2013O\u2013Al avoidance. 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