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Herein, the first high\u2010valent copper(III) trifluoromethyl hydroxide with the tetrameric heterocubane structure [Cu(CF\n                    <jats:sub>3<\/jats:sub>\n                    )\n                    <jats:sub>2<\/jats:sub>\n                    (OH)]\n                    <jats:sub>4<\/jats:sub>\n                    was synthesized by air oxidation of copper(I) in the presence of TMSCF\n                    <jats:sub>3<\/jats:sub>\n                    \/KF and fully characterized, including X\u2010ray crystallography. This unique compound displays versatile reactivity, functioning as a hydroxide base in neutralization reactions with acids, which affords a broad variety of high\u2010valent Cu(III) complexes with two trifluoromethyl groups. The synthetic relevance of copper(III) trifluoromethyl hydroxide for boronic acid trifluoromethylation was demonstrated. The natural population analysis (NPA) charge distribution in the tetrameric heterocubane was studied by DFT calculations, which support the experimentally observed behavior of this compound as a weak hydroxide base, and revealed the positive NPA charge of +1.157 on high\u2010valent copper.\n                  <\/jats:p>","DOI":"10.1002\/chem.202503417","type":"journal-article","created":{"date-parts":[[2025,12,19]],"date-time":"2025-12-19T06:00:12Z","timestamp":1766124012000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":9,"title":["Unprecedented Formation of a Formally Cu(III) Trifluoromethyl Hydroxide Tetramer"],"prefix":"10.1002","volume":"32","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-4951-8113","authenticated-orcid":false,"given":"Vladimir","family":"Motornov","sequence":"first","affiliation":[{"name":"Freie Universit\u00e4t Berlin  Berlin 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