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Despite progress toward optimized efficiency, hurdles persist in steering oxidation products away from environmentally unfriendly products, mostly due to a lack of understanding of structure\u2010selectivity relationships. In this study, the UOR performance of Ni and Cu double hydroxides, which show marked differences in their reactivity and selectivity is evaluated. CuCo hydroxides predominantly produce N\n                    <jats:sub>2<\/jats:sub>\n                    , reaching a current density of 20\u00a0mA\u00a0cm\n                    <jats:sub>geo<\/jats:sub>\n                    <jats:sup>\u22122<\/jats:sup>\n                    at 1.04\u00a0V \u2013 250\u00a0mV less than NiCo hydroxides that generate nitrogen oxides. A collection of in\u2010situ spectroscopies and scattering experiments reveal a unique in situ generated Cu\n                    <jats:sup>(2\u2010x)+<\/jats:sup>\n                    \u2010OO\n                    <jats:sup>\u2212\u2022<\/jats:sup>\n                    active sites in CuCo, which initiates nucleophilic substitution of NH\n                    <jats:sub>2<\/jats:sub>\n                    from the amide, leading to N\u2010N coupling between\n                    <jats:sup>*<\/jats:sup>\n                    NH on Co and Cu. In contrast, the formation of nitrogen oxides on NiCo is primarily attributed to the presence of high\u2010valence Ni\n                    <jats:sup>3+<\/jats:sup>\n                    and Ni\n                    <jats:sup>4+<\/jats:sup>\n                    , which facilitates N\u2010H activation. This process, in conjunction with the excessive accumulation of OH\n                    <jats:sup>\u2212<\/jats:sup>\n                    ions on Jahn\u2010Teller (JT) distorted Co sites, leads to the generation of NO\n                    <jats:sub>2<\/jats:sub>\n                    <jats:sup>\u2212<\/jats:sup>\n                    as the primary product. This work underscores the importance of catalyst composition and structural engineering in tailoring innocuous UOR products.\n                  <\/jats:p>","DOI":"10.1002\/adma.202403187","type":"journal-article","created":{"date-parts":[[2024,7,14]],"date-time":"2024-07-14T10:40:37Z","timestamp":1720953637000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":29,"title":["Double Hydroxide Nanocatalysts for Urea Electrooxidation Engineered toward Environmentally Benign Products"],"prefix":"10.1002","volume":"36","author":[{"given":"Yuwei","family":"Yang","sequence":"first","affiliation":[{"name":"School of Chemical Engineering University of New South Wales  Sydney NSW 2052 Australia"},{"name":"Australian Research Council Centre of Excellence in Carbon Science and Innovation University of New South Wales  Sydney NSW 2052 Australia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jodie 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