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Yet, single\u2010electron processes and the use of redox\u2010active ligands in gold chemistry remain largely underexplored. Here, we report the synthesis, isolation, full characterization and first photocatalytic application of Au(III) semiquinone complexes. The latter are easily obtained via one\u2010electron oxidation of Au(III) catecholate precursors. Experimental and DFT studies establish that oxidation occurs at the O^O ligand while the gold center retains its +3 oxidation state. Owing to their square\u2010planar geometry and electron\u2010rich character, Au(III) catecholate complexes readily engage into electron donor\u2013acceptor (EDA) interactions with organic substrates. Upon visible\u2010light irradiation, these EDA adducts undergo photoinduced single\u2010electron transfer, enabling the generation of aryl radicals from aryldiazonium salts. This reactivity translates into efficient photocatalytic C\u2013H arylation of heterocycles under mild conditions, with broad substrate scope and high functional group tolerance. Variation of the redox\u2010active and ancillary ligands provides a simple means to tune the system, enabling catalytic optimization as substantiated with challenging electron\u2010rich aryldiazonium partners. Mechanistically distinct from established gold photoredox systems, this work delineates a new strategy for standalone Au(III)\u2010mediated photoredox catalysis and highlights the broader potential of redox\u2010active ligands in expanding the reactivity landscape of gold complexes.<\/jats:p>","DOI":"10.1002\/anie.9925350","type":"journal-article","created":{"date-parts":[[2026,5,30]],"date-time":"2026-05-30T11:39:47Z","timestamp":1780141187000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Gold(III) Semiquinone Complexes: Synthesis, Structure, and Application in Photocatalysis"],"prefix":"10.1002","volume":"65","author":[{"given":"Miguel A.","family":"Gonz\u00e1lvez","sequence":"first","affiliation":[{"name":"Laboratoire H\u00e9t\u00e9rochimie Fondamentale Et Appliqu\u00e9e (UMR 5069) CNRS\/Universit\u00e9 De Toulouse  Toulouse 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Jos\u00e9","family":"Gamboa\u2010Carballo","sequence":"additional","affiliation":[{"name":"Institut Des Sciences Analytiques Et De Physico\u2010Chimie pour L'environnement Et Les Mat\u00e9riaux (UMR 5254) CNRS\/Universit\u00e9 De Pau et Des Pays de L'adour  H\u00e9lioparc France"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5960-1877","authenticated-orcid":false,"given":"Karinne","family":"Miqueu","sequence":"additional","affiliation":[{"name":"Institut Des Sciences Analytiques Et De Physico\u2010Chimie pour L'environnement Et Les Mat\u00e9riaux (UMR 5254) CNRS\/Universit\u00e9 De Pau et Des Pays de L'adour  H\u00e9lioparc France"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Gy\u00f6rgy","family":"Szal\u00f3ki","sequence":"additional","affiliation":[{"name":"Laboratoire H\u00e9t\u00e9rochimie Fondamentale Et Appliqu\u00e9e (UMR 5069) CNRS\/Universit\u00e9 De Toulouse  Toulouse 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