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A gas-phase uranyl peroxide dimer supported by three 12-crown-4 ether (12C4) ligands, [(UO 2 ) 2 (O 2 )(12C4) 3 )] 2+ ( A ), was prepared by electrospray ionization. Density functional theory (DFT) indicates a structure with two terminal 12C4 and the third 12C4 bridging the uranium centers. Collision induced dissociation (CID) of A resulted in elimination of the bridging 12C4 to yield a uranyl peroxide dimer with two terminal donor ligands, [(12C4)(UO 2 )(O 2 )(UO 2 )(12C4)] 2+ ( B ). Remarkably, CID of B resulted in elimination of the bridging peroxide concomitant with reduction of U(VI) to U(V) in C , [(12C4)(UO 2 )(UO 2 )(12C4)] 2+ . DFT studies indicate that in C here is direct interaction between the two UO 2  + species, which can thus be considered as a so-called cation-cation interaction (CCI). This formal CCI, induced by tetradentate 12C4 ligands, corresponds to destruction of the linear uranyl moieties and creation of bridging U-O-U oxo-bonds. On the basis of the structural rearrangement to achieve the structurally extreme CCI interaction, it is predicted also to be accessible for PaO 2  + but is less feasible for transuranic actinyls.

Destruction of the Uranyl Moiety in a U(V) “Cation–Cation” Interaction