Investigating the impact of heteroatom alloying extents on regulating the cluster structures is crucial for the fabrication of cluster-based nanomaterials with customized properties. Herein, two structurally comparable PdAu ( = 1, 2) nanoclusters with a uniform surface environment but completely distinct kernel configurations were controllably synthesized and structurally determined. The single Pd-alloyed Pd1Au12 nanocluster retained an icosahedral metal framework, while the Pd2Au12 nanocluster with two Pd heteroatoms exhibited a unique toroidal configuration. The additional Pd heteroatom not only led to significant changes in the cluster frameworks but also profoundly affected their electrocatalytic CO reduction performance. The Pd1Au12 nanocluster demonstrated enhanced catalytic performance, exhibiting a higher current density, a lower onset potential, and greater CO faradaic efficiency compared to the Pd2Au12 nanocluster. This work offers new insights into the customization of the structures and properties of gold nanoclusters by regulating the doping degree of Pd heteroatoms.
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