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Herein, we report the efficient oxidation of benzylic C\u2212H groups in a broad range of substrates under mild conditions over a robust metal\u2013organic framework material, MFM\u2010170, incorporating redox\u2010active [Cu\n                    <jats:sub>2<\/jats:sub>\n                    <jats:sup>II<\/jats:sup>\n                    (O\n                    <jats:sub>2<\/jats:sub>\n                    CR)\n                    <jats:sub>4<\/jats:sub>\n                    ] paddlewheel nodes. A comprehensive investigation employing electron paramagnetic resonance (EPR) spectroscopy and synchrotron X\u2010ray diffraction has identified the critical role of the paddlewheel moiety in activating the oxidant\n                    <jats:sup>t<\/jats:sup>\n                    BuOOH (tert\u2010butyl hydroperoxide) via partial reduction to [Cu\n                    <jats:sup>II<\/jats:sup>\n                    Cu\n                    <jats:sup>I<\/jats:sup>\n                    (O\n                    <jats:sub>2<\/jats:sub>\n                    CR)\n                    <jats:sub>4<\/jats:sub>\n                    ] species.\n                  <\/jats:p>","DOI":"10.1002\/anie.202102313","type":"journal-article","created":{"date-parts":[[2021,4,13]],"date-time":"2021-04-13T21:10:24Z","timestamp":1618348224000},"page":"15243-15247","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":50,"title":["The Origin of Catalytic Benzylic C\u2212H Oxidation over a Redox\u2010Active Metal\u2013Organic Framework"],"prefix":"10.1002","volume":"60","author":[{"given":"Louis","family":"Kimberley","sequence":"first","affiliation":[{"name":"Department of Chemistry University of Manchester  Manchester M13 9PL UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6190-5944","authenticated-orcid":false,"given":"Alena M.","family":"Sheveleva","sequence":"additional","affiliation":[{"name":"Department of Chemistry University of Manchester  Manchester M13 9PL UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jiangnan","family":"Li","sequence":"additional","affiliation":[{"name":"Department of Chemistry University of Manchester  Manchester M13 9PL UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Joseph H.","family":"Carter","sequence":"additional","affiliation":[{"name":"Department of Chemistry University of Manchester  Manchester M13 9PL UK"},{"name":"Diamond Light Source  Harwell Science Campus Oxfordshire OX11 0DE UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xinchen","family":"Kang","sequence":"additional","affiliation":[{"name":"Department of Chemistry University of Manchester  Manchester M13 9PL UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Gemma L.","family":"Smith","sequence":"additional","affiliation":[{"name":"Department of Chemistry University of Manchester  Manchester M13 9PL UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xue","family":"Han","sequence":"additional","affiliation":[{"name":"Department of Chemistry University of Manchester  Manchester M13 9PL UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Sarah J.","family":"Day","sequence":"additional","affiliation":[{"name":"Diamond Light Source  Harwell Science Campus Oxfordshire OX11 0DE UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chiu C.","family":"Tang","sequence":"additional","affiliation":[{"name":"Diamond Light Source  Harwell Science Campus Oxfordshire OX11 0DE UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Floriana","family":"Tuna","sequence":"additional","affiliation":[{"name":"Department of Chemistry University of Manchester  Manchester M13 9PL UK"},{"name":"Photon Science Institute University of Manchester  Manchester M13 9PL UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Eric J. 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