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Photocatalytic urea synthesis from N2, CO2, and H2O offers a sustainable alternative, but efficient C\u2013N coupling is fundamentally limited by the trade-off between intermediate stability and surface migration needed for efficient C\u2013N coupling processes. Strong adsorption of intermediates limits diffusion, whereas weak adsorption causes premature desorption, restricting the C\u2013N coupling efficiency. Facet and spin-state engineering provide a promising route to balance intermediate stabilization, mobility, and interfacial charge transfer. Herein, we prepared oxygen-deficient WOx (x = 2.33\u20132.90) photocatalysts, including nanorods (WO2.33(100)) and nanosheets (WO2.90(001)), by a facile hydrothermal and plasma-treatment method. WO2.33(100) delivered a high photocatalytic urea production rate of 1451.38 \u03bcg g\u20131 h\u20131 under UV irradiation (\u03bb = 365 nm) in a microflow reactor, representing a 3.2-fold enhancement over WO2.90(001) and ranking among the most efficient urea-synthesis photocatalysts reported to date. Mechanistic studies, including isotope labeling, in situ ATR-FTIR, and DFT calculations, reveal that facet-confined oxygen vacancies stabilize low-spin WIII (d3) centers, which simultaneously optimize N2 adsorption while preserving the surface mobility of *NO intermediates, thereby enabling efficient C\u2013N coupling. This work establishes a facet-confined oxygen-vacancy strategy for spin-state regulation of surface intermediates and C\u2013N coupling pathways, providing a general strategy for improved photocatalytic urea synthesis for smart agriculture.<\/jats:p>","DOI":"10.1021\/jacs.6c09316","type":"journal-article","created":{"date-parts":[[2026,9,1]],"date-time":"2026-09-01T16:59:22Z","timestamp":1788281962000},"page":"44116-44127","source":"Crossref","is-referenced-by-count":0,"title":["Enhanced Photocatalytic\nC\u2013N Coupling by Synergistic\nFacet and Spin-State Modulation in Mixed-Valent WO\n                    <i>x<\/i>"],"prefix":"10.1021","volume":"148","author":[{"given":"Shaoquan","family":"Li","sequence":"first","affiliation":[{"name":"Beijing University of Chemical Technology , , ,","place":["Beijing, China, 100029"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shanshan","family":"Wu","sequence":"additional","affiliation":[{"name":"Beijing University of Chemical Technology , , ,","place":["Beijing, China, 100029"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Wenli","family":"Su","sequence":"additional","affiliation":[{"name":"Center for Advanced Quantum Studies Beijing Normal University , , ,","place":["Beijing, China, 100875"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zixian","family":"Li","sequence":"additional","affiliation":[{"name":"Beijing University of Chemical Technology , , ,","place":["Beijing, China, 100029"]},{"name":"ShanghaiTech University , , ,","place":["Shanghai, China, 200000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jinhao","family":"Li","sequence":"additional","affiliation":[{"name":"Beijing University of Chemical Technology , , ,","place":["Beijing, China, 100029"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3296-3093","authenticated-orcid":true,"given":"Geoffrey I.N.","family":"Waterhouse","sequence":"additional","affiliation":[{"name":"The University of Auckland , , ,","place":["Auckland, New Zealand, 1142"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3063-6184","authenticated-orcid":true,"given":"Lihong","family":"Liu","sequence":"additional","affiliation":[{"name":"College of Chemistry Beijing Normal University , , ,","place":["Beijing, China, 100875"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9574-6272","authenticated-orcid":true,"given":"Wenkai","family":"Zhang","sequence":"additional","affiliation":[{"name":"Center for Advanced Quantum Studies Beijing Normal University , , ,","place":["Beijing, China, 100875"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8054-8751","authenticated-orcid":true,"given":"Dermot","family":"O\u2019Hare","sequence":"additional","affiliation":[{"name":"University of Oxford , , Mansfield Road , ,","place":["Oxford, United Kingdom, OX1 3TA"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5325-8991","authenticated-orcid":true,"given":"Yufei","family":"Zhao","sequence":"additional","affiliation":[{"name":"Beijing University of Chemical Technology , , ,","place":["Beijing, China, 100029"]},{"name":"Quzhou Institute for Innovation in Resource Chemical Engineering , , ,","place":["Quzhou, Zhejiang, China, 323000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xue","family":"Duan","sequence":"additional","affiliation":[{"name":"Beijing University of Chemical Technology , , ,","place":["Beijing, China, 100029"]},{"name":"Quzhou Institute for Innovation in Resource Chemical Engineering , , ,","place":["Quzhou, Zhejiang, China, 323000"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,8,27]]},"reference":[{"key":"2026102111070625800_cit1","doi-asserted-by":"publisher","DOI":"10.1002\/ange.202110158","article-title":"Solar Urea: Towards a Sustainable\nFertilizer Industry","volume":"61","author":"Xia","year":"2022","journal-title":"Angew. 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Chem."},{"issue":"8","key":"2026102111070625800_cit36","doi-asserted-by":"publisher","first-page":"6914","DOI":"10.1021\/jacs.4c17444","article-title":"Engineering the Lewis\nAcidity of\nFe Single-Atom Sites via Atomic-Level Tuning of Spatial Coordination\nConfiguration for Enhanced Oxygen Reduction","volume":"147","author":"Qu","year":"2025","journal-title":"J. Am. Chem. Soc."},{"key":"2026102111070625800_cit37","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202312076","article-title":"Photocatalytic Co-Reduction of N2 and CO2 with\nCeO2 Catalyst for Urea Synthesis","volume":"62","author":"Yang","year":"2023","journal-title":"Angew. Chem., Int. Ed."},{"key":"2026102111070625800_cit38","doi-asserted-by":"publisher","DOI":"10.1002\/adfm.202527886","article-title":"Hydrogen Peroxide Electrosynthesis\nUnder Weak Thermodynamic Driving Conditions Enabled by In Situ Spin-State\nTailoring","volume":"36","author":"An","year":"2026","journal-title":"Adv. Funct. Mater."},{"issue":"32","key":"2026102111070625800_cit39","doi-asserted-by":"publisher","first-page":"16204","DOI":"10.1021\/acs.jpcc.3c03991","article-title":"Electron and Hole Polaron Formation and Transport in Monoclinic WO3 Studied by Hybrid Functional Approach","volume":"127","author":"Tao","year":"2023","journal-title":"J. Phys. Chem. C"},{"issue":"5","key":"2026102111070625800_cit40","doi-asserted-by":"publisher","first-page":"2154","DOI":"10.1039\/D4CS00317A","article-title":"Optimizing\nphotocatalysis via electron spin control","volume":"54","author":"He","year":"2025","journal-title":"Chem.\nSoc. Rev."},{"issue":"50","key":"2026102111070625800_cit41","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202313172","article-title":"Rapid Charge Transfer Endowed by\nInterfacial Ni-O Bonding in S-scheme Heterojunction for Efficient\nPhotocatalytic H2 and Imine Production","volume":"62","author":"He","year":"2023","journal-title":"Angew. Chem., Int. 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Interfaces"},{"issue":"5","key":"2026102111070625800_cit44","doi-asserted-by":"publisher","first-page":"3446","DOI":"10.1021\/acscatal.3c05876","article-title":"Ultrathin and Conformal TiOx Overlayers\non WO3 Photoelectrodes for Simultaneous Surface\nTrap Passivation and Heterojunction Formation","volume":"14","author":"Wang","year":"2024","journal-title":"ACS Catal"},{"issue":"29","key":"2026102111070625800_cit45","doi-asserted-by":"publisher","first-page":"16009","DOI":"10.1002\/anie.202102983","article-title":"The Hole-Tunneling\nHeterojunction of Hematite-Based Photoanodes Accelerates Photosynthetic\nReaction","volume":"60","author":"Zhang","year":"2021","journal-title":"Angew. Chem., Int. 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