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Electrocatalytic C\u2500C coupling of biomass molecules followed by hydrodeoxygenation (HDO) offers a cleaner pathway, yet has been limited to dimer formation. Here, we successfully resolved this longstanding bottleneck through construction of Pd\n                    <jats:sub>1<\/jats:sub>\n                    Cu single\u2010atom alloy electrocatalyst, a trimer of 5\u2010hydroxymethylfurfural is obtained with 44.7% selectivity. The combined oligomer (dimer and trimer) selectivity reaches 95.0% with 93.2% Faradaic efficiency, production rate achieves a record high of \u223c50\u00a0g\u00a0g\n                    <jats:sub>cat<\/jats:sub>\n                    <jats:sup>\u22121<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    . Subsequent HDO converts the oligomers into heteroatom\u2010free n\u2010dodecane and n\u2010octadecane diesel blendstocks. Operando spectroscopy reveals a surface\u2010confined ketyl\u2010radical pathway in which isolated Pd atoms regulate hydrogen\u2010atom supply and substrate adsorption, favoring C\u2500C coupling over hydrogenation. This work establishes an electricity\u2010driven route for controlled carbon\u2010chain growth from biomass platforms.\n                  <\/jats:p>","DOI":"10.1002\/anie.3493135","type":"journal-article","created":{"date-parts":[[2026,8,6]],"date-time":"2026-08-06T11:43:37Z","timestamp":1786016617000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Electrocatalytic C\u2013C Coupled Oligomerization From Biomass Molecules Through Pd Single\u2010Atom Interfacial Regulation"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-7389-9860","authenticated-orcid":false,"given":"Shaowei","family":"Yang","sequence":"first","affiliation":[{"name":"Xi'an Key Laboratory of Functional Organic Porous Materials School of Chemistry and Chemical Engineering Northwestern Polytechnical University  Xi'an P. R. 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