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Herein, we pioneer a chlorine radical\u2010mediated strategy to redirect the photocatalytic reaction pathway for methanol conversion toward ethylene glycol (EG). Efficient C\u2500H bond activation is achieved by constructing a Z\u2010scheme heterojunction photocatalyst (ZnIn\n                    <jats:sub>2<\/jats:sub>\n                    S\n                    <jats:sub>4<\/jats:sub>\n                    \/TiO\n                    <jats:sub>2<\/jats:sub>\n                    \u2010Cl) composed of chlorinated TiO\n                    <jats:sub>2<\/jats:sub>\n                    (TiO\n                    <jats:sub>2<\/jats:sub>\n                    \u2010Cl) and ZnIn\n                    <jats:sub>2<\/jats:sub>\n                    S\n                    <jats:sub>4<\/jats:sub>\n                    with efficient charge separation. Photogenerated holes in this system preferentially oxidize surface\u2010adsorbed Cl\n                    <jats:sup>\u2212<\/jats:sup>\n                    to chlorine radicals (Cl\u2022). These radicals drive a thermodynamically favorable hydrogen atom transfer via hydrogen abstraction, cleaving the C\u2500H bond of methanol to form hydroxymethyl radicals (\u2022CH\n                    <jats:sub>2<\/jats:sub>\n                    OH). Subsequent C\u2500C coupling of \u2022CH\n                    <jats:sub>2<\/jats:sub>\n                    OH intermediates, synergistically combined with a self\u2010sustaining Cl\n                    <jats:sup>\u2212<\/jats:sup>\n                    \/Cl\u2022 cycle, produces EG with exceptional selectivity (96.7%) and yield (21.6\u00a0mmol g\n                    <jats:sup>\u22121<\/jats:sup>\n                    ) while suppressing overoxidation. In contrast, nonchlorinated catalysts predominantly utilize photogenerated holes for O\u2500H bond cleavage under identical conditions, yielding only C\n                    <jats:sub>1<\/jats:sub>\n                    products (HCHO, HCOOH). This work not only establishes a solar\u2010driven approach for methanol valorization but also advances mechanistic insights into radical\u2010mediated pathway control in heterogeneous photocatalysis.\n                  <\/jats:p>","DOI":"10.1002\/anie.202510993","type":"journal-article","created":{"date-parts":[[2025,6,12]],"date-time":"2025-06-12T03:08:05Z","timestamp":1749697685000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":19,"title":["Chlorine Radical\u2010Mediated Photocatalytic C\u2500C Coupling of Methanol to Ethylene Glycol with Near\u2010Unity Selectivity"],"prefix":"10.1002","volume":"64","author":[{"given":"Guang\u2010Xing","family":"Dong","sequence":"first","affiliation":[{"name":"Institute for New Energy Materials and Low Carbon Technologies School of Chemistry and Chemical Engineering Tianjin University of Technology  Tianjin 300384 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Meng\u2010Ran","family":"Zhang","sequence":"additional","affiliation":[{"name":"Institute for New Energy Materials and Low Carbon Technologies School of Chemistry and Chemical Engineering Tianjin University of Technology  Tianjin 300384 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Su\u2010Xian","family":"Yuan","sequence":"additional","affiliation":[{"name":"Institute for New Energy Materials and Low Carbon Technologies School of Chemistry and Chemical Engineering Tianjin University of Technology  Tianjin 300384 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0275-9497","authenticated-orcid":false,"given":"Min","family":"Zhang","sequence":"additional","affiliation":[{"name":"Institute for New Energy Materials and Low Carbon Technologies School of Chemistry and Chemical Engineering Tianjin University of Technology  Tianjin 300384 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Tong\u2010Bu","family":"Lu","sequence":"additional","affiliation":[{"name":"Institute for New Energy Materials and Low Carbon Technologies School of Chemistry and Chemical Engineering Tianjin University of Technology  Tianjin 300384 China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2025,6,18]]},"reference":[{"key":"e_1_2_5_1_1","doi-asserted-by":"publisher","DOI":"10.1039\/D4CS00551A"},{"key":"e_1_2_5_2_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.accounts.3c00187"},{"key":"e_1_2_5_3_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41563-023-01519-y"},{"key":"e_1_2_5_4_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.accounts.3c00551"},{"key":"e_1_2_5_5_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41929-023-00927-2"},{"key":"e_1_2_5_6_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202314288"},{"key":"e_1_2_5_7_1","doi-asserted-by":"publisher","DOI":"10.1126\/sciadv.ads4018"},{"key":"e_1_2_5_8_1","doi-asserted-by":"publisher","DOI":"10.1021\/acscatal.3c04941"},{"key":"e_1_2_5_9_1","doi-asserted-by":"publisher","DOI":"10.1021\/acscatal.4c01596"},{"key":"e_1_2_5_10_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41929-022-00808-0"},{"key":"e_1_2_5_11_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-024-46232-9"},{"key":"e_1_2_5_12_1","doi-asserted-by":"publisher","DOI":"10.1039\/D1CC07276E"},{"key":"e_1_2_5_13_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-024-52999-8"},{"key":"e_1_2_5_14_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-018-03543-y"},{"key":"e_1_2_5_15_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202402004"},{"key":"e_1_2_5_16_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.chempr.2019.01.005"},{"key":"e_1_2_5_17_1","doi-asserted-by":"publisher","DOI":"10.1002\/cctc.201900437"},{"key":"e_1_2_5_18_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.jhazmat.2019.120822"},{"key":"e_1_2_5_19_1","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.3c06688"},{"key":"e_1_2_5_20_1","author":"Chen G.","year":"2025","journal-title":"Angew. 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