Abstract
AbstractThe uranyl cage clusters (UO2)22(O2)15(PHO3)20(H2O)1026– (U22) and (UO2)28(O2)20(PHO3)24(H2O)1232– (U28) can be probed in aqueous solutions by using a combination of 1H Diffusion‐Ordered Spectroscopy (DOSY) and 1H‐31P Heteronuclear‐Single Quantum Coherence (HSQC) spectroscopy. This class of clusters is ideal for 1H NMR analysis in D2O because of the covalent character of the H–P bond in the phosphonic bridges. 1H DOSY indicates that the clusters are stable in solution and provides hydrodynamic radii of 9.8 ± 0.4 Å for the U22 and 12.3 ± 0.5 Å for the U28 clusters. Furthermore, 1H‐31P HSQC delivers unequivocal signal assignment for both nuclei, which enables solution dynamics to be monitored by variable‐temperature experiments, and reveals the presence of phosphonic‐bridge conformers. The results provide some of the first dynamic information about steady conformational changes in these enormous actinide macroions.
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