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The crystal structure recorded at 10\u2005K after blue light irradiation reveals an heptacoordinated Mo(CN)<jats:sub>7<\/jats:sub> species originating from the light\u2010induced cleavage of one Mo\u2212CN bond, concomitant with the photoinduced formation of a paramagnetic signal. When this complex is heated to 70\u2005K, it returns to its original diamagnetic ground state, demonstrating full reversibility. The photomagnetic properties show a partial conversion into a triplet state possessing significant magnetic anisotropy, which is in agreement with theoretical studies. Inspired by these results, we isolated the new compound [K(crypt\u2010222)]<jats:sub>3<\/jats:sub>[Mo<jats:sup>IV<\/jats:sup>(CN)<jats:sub>7<\/jats:sub>]\u22c53\u2009CH<jats:sub>3<\/jats:sub>CN using a photochemical pathway, confirming that photodissociation leads to a stable heptacyanomolybdate(IV) species in solution.<\/jats:p>","DOI":"10.1002\/anie.201914527","type":"journal-article","created":{"date-parts":[[2019,12,3]],"date-time":"2019-12-03T06:39:11Z","timestamp":1575355151000},"page":"3117-3121","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":42,"title":["Photoinduced Mo\u2212CN Bond Breakage in Octacyanomolybdate Leading to Spin Triplet Trapping"],"prefix":"10.1002","volume":"59","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-6233-356X","authenticated-orcid":false,"given":"Xinghui","family":"Qi","sequence":"first","affiliation":[{"name":"CNRS Univ. 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