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An intriguing feature of these complexes is the difference in the structure of a pair of silsesquioxane ligands despite identical (Cu<jats:sub>6<\/jats:sub>) nuclearity and number (four) of acetate fragments. Formation of particular combination of silsesquioxane ligands (cyclic\/cyclic <jats:italic>vs<\/jats:italic> condensed\/condensed <jats:italic>vs<\/jats:italic> cyclic\/condensed) was found to be dependent on the synthesis\/crystallization media. A combination of Si<jats:sub>4<\/jats:sub>\u2010cyclic and Si<jats:sub>6<\/jats:sub>\u2010condensed silsesquioxane ligands is a brand new feature of cage metallasilsesquioxanes. A representative Cu<jats:sub>6<\/jats:sub>\u2010complex (<jats:bold>4<\/jats:bold>) (with cyclic silsesquioxanes) exhibited high catalytic activity in the oxidation of alkanes and alcohols with peroxides. Maximum yield of the products of cyclohexane oxidation attained 30\u2009%. The compound <jats:bold>4<\/jats:bold> was also tested as catalyst in the Baeyer\u2010Villiger oxidation of cyclohexanone by <jats:italic>m\u2010<\/jats:italic>chloroperoxybenzoic acid: maximum yields of 88\u2009% and 100\u2009% of \u03f5\u2010caprolactone were achieved upon conventional heating at 50\u2009\u00b0C for 4\u2005h and MW irradiation at 70 or 80\u2009\u00b0C during 30\u2005min, respectively. It was also possible to obtain the lactone (up to 16\u2009% yield) directly from the cyclohexane via a tandem oxidation\/Baeyer\u2010Villiger oxidation reaction using the same oxidant.<\/jats:p>","DOI":"10.1002\/chem.202401164","type":"journal-article","created":{"date-parts":[[2024,3,29]],"date-time":"2024-03-29T09:55:39Z","timestamp":1711706139000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":9,"title":["A Family of Hexacopper Phenylsilsesquioxane\/Acetate Complexes: Synthesis, Solvent\u2010Controlled Cage Structures, and Catalytic Activity"],"prefix":"10.1002","volume":"30","author":[{"given":"Anna Y.","family":"Zueva","sequence":"first","affiliation":[{"name":"A.N. 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