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suppressing the formation of three\u2010dimensional (3D) Pd frameworks. Here, we show that anti\u2010galvanic incorporation of antimony (Sb), a p\u2010block congener of phosphorus, selectively perturbs planar Pd\u2500S coordination while preserving Pd\u2500Pd connectivity. Sb acts as a dimensional regulator that enables the formation of stable, 3D Pd\u2500Sb nanoclusters with atomic precision, as exemplified by the successful synthesis of the [Pd\n                    <jats:sub>13<\/jats:sub>\n                    Sb\n                    <jats:sub>2<\/jats:sub>\n                    (PPh\n                    <jats:sub>3<\/jats:sub>\n                    )\n                    <jats:sub>2<\/jats:sub>\n                    (S\u2010Adm)\n                    <jats:sub>10<\/jats:sub>\n                    ] (denoted as Pd\n                    <jats:sub>13<\/jats:sub>\n                    Sb\n                    <jats:sub>2<\/jats:sub>\n                    ) nanocluster. Single\u2010crystal X\u2010ray diffraction (SCXRD) analysis unveiled a unique 3D metal kernel, a structural feature not previously reported in thiolated Pd nanoclusters. When applied to the semihydrogenation of phenylacetylene, the Pd\n                    <jats:sub>13<\/jats:sub>\n                    Sb\n                    <jats:sub>2<\/jats:sub>\n                    catalyst exhibited excellent catalytic performance. Density functional theory calculations indicate that the synergistic Pd\u2500Sb dual\u2010site architecture not only facilitates H\n                    <jats:sub>2<\/jats:sub>\n                    activation but also optimizes the binding energy of intermediates, ensuring preferential styrene desorption and thus suppressing over\u2010hydrogenation. These results establish Sb\u2010enabled dimensional control to overcome intrinsic structural limitations in palladium nanoclusters and to unlock their catalytic potentials.\n                  <\/jats:p>","DOI":"10.1002\/adma.73523","type":"journal-article","created":{"date-parts":[[2026,6,16]],"date-time":"2026-06-16T10:25:00Z","timestamp":1781605500000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["Sb\u2010Enabled Dimensional Reprogramming of Palladium Nanoclusters for Enhanced Catalysis"],"prefix":"10.1002","volume":"38","author":[{"given":"Qihang","family":"Wang","sequence":"first","affiliation":[{"name":"Key Laboratory of Materials Physics Anhui Key Laboratory of Nanomaterials and Nanotechnology CAS Center for Excellence in Nanoscience Institute of Solid State Physics HFIPS Chinese Academy of Sciences  Hefei P. R. 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