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Herein, alkyl thiols (C\n                    <jats:sub>9<\/jats:sub>\n                    SH) were site\u2011specifically grafted onto Au sites supported on planar TiO\n                    <jats:sub>2<\/jats:sub>\n                    , forming the archetypal C\n                    <jats:sub>9<\/jats:sub>\n                    S\u2010Au\n                    <jats:sup>\u03b4+<\/jats:sup>\n                    \/Au\/TiO\n                    <jats:sub>2<\/jats:sub>\n                    system featuring covalent gold\u2010thiolate interplay. Combined experimental and theoretical analyses revealed that covalent Au\u2010thiolate interaction could modulate the interfacial electronic structure and upshift the\n                    <jats:italic>d<\/jats:italic>\n                    \u2011band center of Au sites, thereby strengthening *CH\n                    <jats:sub>3<\/jats:sub>\n                    adsorption and lowering the C\u2500C coupling barrier, thus suppressing the\n                    <jats:bold>\u00b7<\/jats:bold>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    <jats:sup>\u2212<\/jats:sup>\n                    \u2010driven overoxidation. Moreover, the reconstructed C\n                    <jats:sub>9<\/jats:sub>\n                    S\u2010Au\n                    <jats:sup>\u03b4+<\/jats:sup>\n                    sites acted as rapid electron extraction channels, drawing electrons from adjacent Au nanoparticles and preserving long\u2010lived photogenerated holes for C\u2500H activation. Meanwhile, the alkyl chains served as \u201cmolecular fences\u201d, effectively promoting local CH\n                    <jats:sub>4<\/jats:sub>\n                    enrichment and stabilizing *CH\n                    <jats:sub>3<\/jats:sub>\n                    intermediates. The optimized C\n                    <jats:sub>9<\/jats:sub>\n                    S\u2010Au\n                    <jats:sup>\u03b4+<\/jats:sup>\n                    \/Au\/TiO\n                    <jats:sub>2<\/jats:sub>\n                    photocatalyst exhibited an excellent yield of 22.92\u00a0mmol g\n                    <jats:sub>cat<\/jats:sub>\n                    <jats:sup>\u22121<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    for C\n                    <jats:sub>2+<\/jats:sub>\n                    products with 93.9% selectivity, ranking it among the state\u2010of\u2010the\u2010art noble\u2010metal\u2010loaded photocatalysts for POCM. This work establishes site\u2010specific molecular engineering as an effective strategy to regulate interfacial charge redistribution and redirect radical coupling pathways, enabling CH\n                    <jats:sub>4<\/jats:sub>\n                    conversion to multi\u2010carbon products with enhanced activity and selectivity simultaneously.\n                  <\/jats:p>","DOI":"10.1002\/anie.6847901","type":"journal-article","created":{"date-parts":[[2026,9,1]],"date-time":"2026-09-01T10:39:01Z","timestamp":1788259141000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Site\u2010Specific Molecular Engineering Redirects Radical Pathways for Selective Photocatalytic Coupling of Methane to C\n                    <sub>2+<\/sub>\n                    Hydrocarbons"],"prefix":"10.1002","volume":"65","author":[{"given":"Yaru","family":"Shao","sequence":"first","affiliation":[{"name":"State Key Laboratory of Fine Chemical Frontiers Science Center For Smart Materials Oriented Chemical Engineering School of Chemical Engineering Dalian University of Technology  Dalian P. 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