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Here, pulsed oxidative\u2013reductive electrolysis temporally coordinates CO\n                    <jats:sub>2<\/jats:sub>\n                    reduction and NH\n                    <jats:sub>3<\/jats:sub>\n                    oxidation, regulating the generation and coexistence of carbon\u2010 and nitrogen\u2010derived intermediates. Co\/CuNC, containing atomically dispersed Co and Cu sites within a nitrogen\u2010doped carbon (NC), achieves a total C\u2500N faradaic efficiency of 42 \u00b1 4%, dominated by urea (20 \u00b1 2%) and ethyl urea (16 \u00b1 2%), with respective yield rates (YR) of 295 \u00b1 25 and 50 \u00b1 5\u00a0mmol h\n                    <jats:sup>\u22121<\/jats:sup>\n                    g\n                    <jats:sub>cat<\/jats:sub>\n                    <jats:sup>\u22121<\/jats:sup>\n                    . In situ synchrotron x\u2010ray absorption spectroscopy (XAS) reveals potential\u2010dependent changes in Cu and Co oxidation states and coordination environments, while in situ infrared spectroscopy identifies pulse\u2010regulated *CO and *NH\n                    <jats:italic>\n                      <jats:sub>x<\/jats:sub>\n                    <\/jats:italic>\n                    intermediates and suggests concurrent electrochemical and W\u00f6hler\u2010type pathways. Density functional theory calculations reveal complementary site functions: Cu favors *NH\n                    <jats:sub>2<\/jats:sub>\n                    formation, whereas Co more strongly stabilizes *NH\n                    <jats:italic>\n                      <jats:sub>x<\/jats:sub>\n                    <\/jats:italic>\n                    and *CO intermediates, with *CO also accessible at Cu sites. These findings establish temporal coordination of reactant activation, intermediate populations, and active\u2010site states as a mode\u2010enabled strategy for accessing higher\u2010order C\u2500N products.\n                  <\/jats:p>","DOI":"10.1002\/adma.75357","type":"journal-article","created":{"date-parts":[[2026,10,13]],"date-time":"2026-10-13T14:31:28Z","timestamp":1791901888000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Pulsed Oxidative\u2013Reductive Electrolysis Over Dual Cu and Co Single\u2010Atom Sites for Urea Electrosynthesis"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-3241-3382","authenticated-orcid":false,"given":"Putri","family":"Ramadhany","sequence":"first","affiliation":[{"name":"School of Chemical Engineering University of New South Wales  Sydney New South Wales Australia"},{"name":"Center For Renewable Energy Conversion, Chemical Engineering Department, 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