Environmentally Friendly, Photochemical Access to [[Formula: see text] ]Au(III) Pincer Complexes By Oxidative Addition

Starting from commercially available DMSAuCl and diazonium salts, cationic [[Formula: see text] ]Au(III) complexes were synthesized in a selective, photosensitizer‐free, photochemical reaction by irradiation with blue LED light. This new protocol represents the first easy synthesis of these types of pincer complexes in moderate to excellent yield starting from a readily available gold(I) precursor with nitrogen as the only by‐product. Owing to the disadvantages of known protocols, especially the toxicity in the case of a transmetalation with mercury or the necessity for a mostly twofold excess of a gold precursor, this method offers an attractive alternative towards this kind of gold(III) complexes. In addition, the first arylated [[Formula: see text] ]Au(III) pincer complex was synthesized by using this technology.