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Here, we report an MOF-derived cobalt catalyst for the e\u00a0-H of acetone and pyridine. A new two-dimensional cobalt metal\u2013organic framework, Co-L0-NS, composed of Co(II) nodes and polyaromatic carboxylate linkers, was synthesized as nanosheets and used as a precursor to generate the active catalyst under cathodic bias. Electrochemical pretreatment induces controlled framework reconstruction to form MD-Cat, a highly dispersed, structurally disordered, Co(OH)2-rich nanocluster material. MD-Cat catalyzes the e\u00a0-H of acetone to isopropanol with nearly quantitative Faradaic efficiency at optimized potentials and promotes pyridine hydrogenation to piperidine with up to 50% Faradaic efficiency. Comparative studies with electrodeposited cobalt, commercial cobalt nanoparticles, and bulk Co(OH)2 show that the MOF-derived catalyst exhibits superior current densities and product selectivity, which we attribute to its nanoscale morphology and hydroxylated cobalt environment. In situ Co K-edge XAS, XPS, PXRD, ATR-SEIRAS, and STEM analyses indicate that Co remains predominantly in the +2 oxidation state during catalysis while undergoing structural reorganization. Tafel analysis supports a PCET-type mechanism for acetone hydrogenation; while DFT calculations suggest that the Co\/Co(OH)2 interface suppresses HER by weakening H* binding while preserving organic-substrate activation. These results highlight MOF-templated electrochemical reconstruction as a promising approach for designing selective e\u00a0-H catalysts, not only by increasing catalyst accessibility through nanostructuring but also by enabling the formation of unique catalytic motifs that would otherwise be difficult to access using traditional methods.<\/jats:p>","DOI":"10.1021\/jacs.6c11639","type":"journal-article","created":{"date-parts":[[2026,8,4]],"date-time":"2026-08-04T17:02:13Z","timestamp":1785862933000},"page":"35004-35016","source":"Crossref","is-referenced-by-count":0,"title":["Electrocatalytic\nHydrogenation with Nanoparticles\nDerived from a Cobalt Metal\u2013Organic Framework"],"prefix":"10.1021","volume":"148","author":[{"given":"Biki Kumar","family":"Behera","sequence":"first","affiliation":[{"name":"University of Illinois Chicago , , , ,","place":["Chicago, Illinois, United States, 60607"]},{"name":"Argonne National Laboratory , , , ,","place":["Lemont, Illinois, United States, 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