Herein, we report a new salt of a pyrophosphate-functionalized uranyl peroxide nanocluster {UPp} (1) exhibiting O molecular symmetry both in the solid and solution. Study of the system yielding 1 across a wide range of pH by single-crystal X-ray diffraction, small-angle X-ray scattering, and a combination of traditional P and diffusion-ordered spectroscopy (DOSY) NMR affords unprecedented insight into the amphoteric chemistry of this uranyl peroxide system. Key results include formation of a rare binary {U}·{UPp} (3) system observed under alkaline conditions, and evidence of acid-promoted decomposition of {UPp} (1) followed by spatial rearrangement and condensation of {U} building blocks into the {UPp} (2) cluster. Furthermore, P DOSY NMR measurements performed on saturated solutions containing crystalline {UPp} show only trace amounts (∼2% relative abundance) of the intact form of this cluster, suggesting a complex interconversion of {UPp}, {UPp}, and {UPp} ions.
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