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Here, we demonstrate that the decoration of iodine (I) single atoms on ultrathin CN (IUCN) benefit the formation of C\u2550O during vapor\u2010engaged photocatalytic processes, reduces the adsorption capacity of OH species, and strengthens the tri\u2010coordinated bridging nitrogen atoms (C\u2500N\u2550C) linkages, preventing the self\u2010decomposition of IUCN. The formed C\u2500I covalent bond at the IUCN surface provides a direct channel for photogenerated hole transfer, improving the separation of the in\u2010plane electron\u2010hole pairs. Furthermore, orbital hybridization between the N\u20132p orbitals of IUCN and the C\u20132p orbitals of CO\n                    <jats:sub>2<\/jats:sub>\n                    lowers the energy of antibonding orbitals in CO\n                    <jats:sub>2<\/jats:sub>\n                    , enhancing its activation and subsequent transformation. The optimal IUCN photocatalyst achieved CO and CH\n                    <jats:sub>4<\/jats:sub>\n                    yields of 181.09 and 16.27\u00a0\u00b5mol\u00a0g\n                    <jats:sup>\u22121<\/jats:sup>\n                    \u00a0h\n                    <jats:sup>\u22121<\/jats:sup>\n                    under simulated solar light irradiation, respectively. The CO and CH\n                    <jats:sub>4<\/jats:sub>\n                    yields are 90.29 and 17.92\u00a0\u00b5mol\u00a0g\n                    <jats:sup>\u22121<\/jats:sup>\n                    \u00a0h\n                    <jats:sup>\u22121<\/jats:sup>\n                    under visible light irradiation, respectively. This study expands the synthetic approaches for nonmetal single\u2010atom catalysts and offers insights into the relationship between the configuration of single atoms and the reaction pathways.\n                  <\/jats:p>","DOI":"10.1002\/smll.202511394","type":"journal-article","created":{"date-parts":[[2025,12,9]],"date-time":"2025-12-09T14:44:14Z","timestamp":1765291454000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Isolated Iodine Single Atoms Regulating the in\u2010Plane Electronic Structure of G\u2010C\n                    <sub>3<\/sub>\n                    N\n                    <sub>4<\/sub>\n                    for Enhanced CO\n                    <sub>2<\/sub>\n                    Photoreduction"],"prefix":"10.1002","volume":"22","author":[{"given":"Fei","family":"Rao","sequence":"first","affiliation":[{"name":"Quantum Materials and Devices Key Laboratory of Shaanxi Province's High Education Institution, School of Physics and Information Technology Shaanxi Normal University  Xi'an 710062 P. 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China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xianjin","family":"Shi","sequence":"additional","affiliation":[{"name":"State Key Lab of Loess and Quaternary Geology (SKLLQG), Institute of Earth Environment Chinese Academy of Sciences  Xi'an 710061 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Lujun","family":"Zhu","sequence":"additional","affiliation":[{"name":"Quantum Materials and Devices Key Laboratory of Shaanxi Province's High Education Institution, School of Physics and Information Technology Shaanxi Normal University  Xi'an 710062 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xiao\u2010Ming","family":"Chen","sequence":"additional","affiliation":[{"name":"Quantum Materials and Devices Key Laboratory of Shaanxi Province's High Education Institution, School of Physics and Information Technology Shaanxi Normal University  Xi'an 710062 P. R. 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