a significantly high total turnover number (TTO) of approximately 153000 over 8 h was achieved with an excellent turnover frequency (TOF) of 914 min–1 and an activation energy of 28.1 kJ mol–1. Detailed characterization by means of TEM, EDX, H2-TPR, and in situ XAFS measurements revealed that a synergistic alloying effect originates from the random distribution of Ru–Ni nanoparticles with a mean diameter of 2.3 nm and plays a crucial role in the exceptional catalytic performance. This catalytic system has particular potential for industrial application in fuel cells due to advantages such as the facile preparation method, the use of relatively cheap metals, and the exceptionally high catalytic activity.1f:T46e,The design and exploitation of high-performance catalysts have gained considerable attention in selective hydrogenation reactions, but remain a huge challenge. Herein, we report a RuNi single atom alloy (SAA) in which Ru single atoms are anchored onto Ni nanoparticle surface via Ru-Ni coordination accompanied with electron transfer from sub-surface Ni to Ru. The optimal catalyst 0.4% RuNi SAA exhibits simultaneously improved activity (TOF value: 4293 h^-1) and chemoselectivity toward selective hydrogenation of 4-nitrostyrene to 4-aminostyrene (yield: >99%), which is, to the best of our knowledge, the highest level compared with reported heterogeneous catalysts. In situ experiments and theoretical calculations reveal that the Ru-Ni interfacial sites as intrinsic active centers facilitate the preferential cleavage of N-O bond with a decreased energy barrier by 0.28 eV. In addition, the Ru-Ni synergistic catalysis promotes the formation of intermediates (C₈H₇NO* and C₈H₇NOH*) and accelerates the rate-determining step (hydrogenation of C₈H₇NOH*).20:T6dd,

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