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Heterogeneous catalysts based on sub-nanometer metal clusters often exhibitstrongly size-dependent properties, and the addition or removal of a singleatom can make all the difference. Identifying the most active species anddeciphering the reaction mechanism is extremely difficult, however, because itis often not clear how the catalyst evolves in operando. Here, we utilize acombination of atomically resolved scanning probe microscopies, spectroscopictechniques, and density functional theory (DFT)-based calculations to study COoxidation by a model Pt/Fe3O4(001) single-atom catalyst. We demonstrate that(PtCO)2 dimers, formed dynamically through the agglomeration of mobilePt-carbonyl species, catalyse a reaction involving the oxide support to formCO2. Pt2 dimers produce one CO2 molecule before falling apart into two adatoms,releasing the second CO. Interestingly, Olattice extraction only becomes facilewhen both the Pt-dimer and the Fe3O4 support can access metastableconfigurations, suggesting that substantial, concerted rearrangements of bothcluster and support must be considered for reactions occurring at elevatedtemperature.

CO oxidation by Pt2/Fe3O4: metastable dimer and support configurations facilitate lattice oxygen extraction