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As well as full X\u2010ray crystallographic analysis, we studied the reactivity of the cluster using both solution\u2010state NMR spectroscopy and mass spectrometry. These techniques show that the cluster undergoes a structural rearrangement in solution whereby the {HPO<jats:sub>3<\/jats:sub>} moieties dimerize to form a weakly interacting (O<jats:sub>3<\/jats:sub>PH\u22c5\u22c5\u22c5HPO<jats:sub>3<\/jats:sub>) moiety. In the crystalline state the cluster exhibits a thermally triggered oxidation of the two P<jats:sup>III<\/jats:sup> template moieties to form P<jats:sup>V<\/jats:sup>\u2005centers (phosphite to phosphate), commensurate with the transformation of the cage into a Wells\u2013Dawson {W<jats:sub>18<\/jats:sub>O<jats:sub>54<\/jats:sub>} cluster.<\/jats:p>","DOI":"10.1002\/anie.201502295","type":"journal-article","created":{"date-parts":[[2015,5,27]],"date-time":"2015-05-27T16:31:52Z","timestamp":1432744312000},"page":"7895-7899","source":"Crossref","is-referenced-by-count":35,"title":["Following the Reaction of Heteroanions inside a {W<sub>18<\/sub>O<sub>56<\/sub>} Polyoxometalate Nanocage by NMR Spectroscopy and Mass 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