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In order to explain the efficient redox cycling between Cu<jats:sup>II<\/jats:sup>\u2010A<jats:italic>\u03b2<\/jats:italic> (distorted square\u2010pyramidal) and Cu<jats:sup>I<\/jats:sup>\u2010A<jats:italic>\u03b2<\/jats:italic> (digonal) resting states, the existence of a low\u2010populated \u201cin\u2010between\u201d state, prone to bind Cu in both oxidation states, has been postulated. Here, we exploited the partial X\u2010ray induced photoreduction at 10\u2005K, followed by a thermal relaxation at 200\u2005K, to trap and characterize by X\u2010ray Absorption Spectroscopy (XAS) a partially reduced Cu\u2010A<jats:italic>\u03b2<\/jats:italic><jats:sub>1\u201316<\/jats:sub> species different from the resting states. Remarkably, the XAS spectrum is well\u2010fitted by a previously proposed model of the \u201cin\u2010between\u201d state, hence providing the first direct spectroscopic characterization of an intermediate state. The present approach could be used to explore and identify the catalytic intermediates of other relevant metal complexes.<\/jats:p>","DOI":"10.1002\/anie.202217791","type":"journal-article","created":{"date-parts":[[2023,3,4]],"date-time":"2023-03-04T07:40:56Z","timestamp":1677915656000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":15,"title":["Chasing the Elusive \u201cIn\u2010Between\u201d State of the Copper\u2010Amyloid <i>\u03b2<\/i> Complex by X\u2010ray Absorption through Partial Thermal Relaxation after Photoreduction"],"prefix":"10.1002","volume":"62","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-1944-3552","authenticated-orcid":false,"given":"Enrico","family":"Falcone","sequence":"first","affiliation":[{"name":"Institut de Chimie (UMR 7177) University of Strasbourg, CNRS  4 Rue Blaise Pascal 67081 Strasbourg 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