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Herein, a rationally designed Ni\u2013Fe bimetallic pyromellitic acid polymer catalyst (Ni\u2010PMDA@Fe) is developed for efficient urea electrosynthesis. This metal\u2013organic polymer provides structural robustness, abundant active sites, and a tunable coordination environment, optimizing C\u2013N coupling kinetics. Ni\u2010PMDA@Fe achieves a urea yield of 449.56\u2009mg\u2009h\n                    <jats:sup>\u22121<\/jats:sup>\n                    \u2009g\n                    <jats:sub>cat<\/jats:sub>\n                    <jats:sup>\u22121<\/jats:sup>\n                    and a Faradaic efficiency (FE) of 41.06% at \u20130.5\u2009V\n                    <jats:sub>RHE<\/jats:sub>\n                    , significantly surpassing monometallic controls (Ni\u2010BDC, Ni\u2010PMDA). Fe incorporation modulates the electronic structure of Ni, enhances charge transfer, and stabilizes key reaction intermediates, enabling synergistic NO\n                    <jats:sub>3<\/jats:sub>\n                    <jats:sup>\u2212<\/jats:sup>\n                    \/CO\n                    <jats:sub>2<\/jats:sub>\n                    coupling. Comprehensive characterization confirms homogeneous Fe doping and a dual\u2010metal\u2010site configuration. Unlike single\u2010atom or monometallic systems, the Ni\u2013Fe dual\u2010site architecture optimally tunes the adsorption kinetics of critical intermediates. The catalyst maintains a FE exceeding 30% over a 30\u2009h stability test, demonstrating robust operational stability. Furthermore, techno\u2010economic analysis (TEA) indicates competitive production costs when powered by renewable energy, highlighting scalability potential. This word demonstrates a practical pathway for sustainable urea synthesis by converting pollutants (NO\n                    <jats:sub>3<\/jats:sub>\n                    <jats:sup>\u2212<\/jats:sup>\n                    \/CO\n                    <jats:sub>2<\/jats:sub>\n                    ) into value\u2010added product, thereby contributing to decarbonizing fertilizer production and mitigating nitrogen pollution.\n                  <\/jats:p>","DOI":"10.1002\/cssc.202502676","type":"journal-article","created":{"date-parts":[[2026,3,13]],"date-time":"2026-03-13T00:01:27Z","timestamp":1773360087000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["Ni\u2013Fe Dual\u2010Site Polymer Catalyst for High Performance and Stable Electrochemical Urea Synthesis from CO\n                    <sub>2<\/sub>\n                    and NO\n                    <sub>3<\/sub>\n                    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