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Herein, a rapid construction of novel BF<jats:sub>2<\/jats:sub> complexes with N,O\u2010bidentate ligands by using Cu(BF<jats:sub>4<\/jats:sub>)<jats:sub>2<\/jats:sub>\u20226H<jats:sub>2<\/jats:sub>O as a catalyst and BF<jats:sub>2<\/jats:sub> source is disclosed, which avoids the need for pre\u2010composing the N,O\u2010bidentate ligands and features a broad substrate scope and a high tolerance level for sensitive functional groups. Moreover, molecular oxygen is employed as the terminal oxidant in this transformation. A library of 36 compounds as a new class of BF<jats:sub>2<\/jats:sub> complexes with remarkable photophysical properties is delivered in good to excellent yields, showing a substituent\u2010dependency on the photophysical properties, derived from the <jats:italic>\u03c0<\/jats:italic>\u2013<jats:italic>\u03c0<\/jats:italic>* character of the photoexcited state. In addition, aggregation\u2010induced emission (AIE) is observed and quantified for the brightest exemplars. The excited state properties are fully investigated in solids and in THF\/H<jats:sub>2<\/jats:sub>O mixtures. Hence, a new series of photofunctional materials with variable photophysical properties is reported, with potential applications for sensing, bioimaging, and optoelectronics.<\/jats:p>","DOI":"10.1002\/advs.202101814","type":"journal-article","created":{"date-parts":[[2021,7,26]],"date-time":"2021-07-26T06:10:41Z","timestamp":1627279841000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":27,"title":["AIE\u2010Active Difluoroboron Complexes with N,O\u2010Bidentate Ligands: Rapid Construction by Copper\u2010Catalyzed C\u2212H Activation"],"prefix":"10.1002","volume":"8","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-3648-8039","authenticated-orcid":false,"given":"Guangying","family":"Tan","sequence":"first","affiliation":[{"name":"Organisch\u2010Chemisches Institut Westf\u00e4lische Wilhelms\u2010Universit\u00e4t M\u00fcnster  Corrensstra\u00dfe 40 M\u00fcnster 48149 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