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This new synthetic approach is exemplified by the synthesis and characterization of the heteroleptic complexes, <jats:italic>trans<\/jats:italic>\u2010[M<jats:sup>IV<\/jats:sup>F<jats:sub>4<\/jats:sub>(CN)<jats:sub>2<\/jats:sub>]<jats:sup>2\u2212<\/jats:sup> (M=Re, Os), obtained from their homoleptic [M<jats:sup>IV<\/jats:sup>F<jats:sub>6<\/jats:sub>]<jats:sup>2\u2212<\/jats:sup> parents. As shown by combined high\u2010field electron paramagnetic resonance spectroscopy and magnetization measurements, the partial substitution of fluoride by cyanide ligands leads to a marked increase in the magnetic anisotropy of <jats:italic>trans<\/jats:italic>\u2010[ReF<jats:sub>4<\/jats:sub>(CN)<jats:sub>2<\/jats:sub>]<jats:sup>2\u2212<\/jats:sup> as compared to [ReF<jats:sub>6<\/jats:sub>]<jats:sup>2\u2212<\/jats:sup>, reflecting the severe departure from an ideal octahedral (O<jats:sub>h<\/jats:sub> point group) ligand field. This methodology paves the way toward the realization of new heteroleptic transition metal complexes that may be used as highly anisotropic building\u2010blocks for the design of high\u2010performance molecule\u2010based magnetic materials.<\/jats:p>","DOI":"10.1002\/anie.201914934","type":"journal-article","created":{"date-parts":[[2020,2,21]],"date-time":"2020-02-21T09:41:35Z","timestamp":1582278095000},"page":"10306-10310","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":14,"title":["Access to Heteroleptic Fluorido\u2010Cyanido Complexes with a Large Magnetic Anisotropy by Fluoride Abstraction"],"prefix":"10.1002","volume":"59","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-5811-6300","authenticated-orcid":false,"given":"Jun\u2010Liang","family":"Liu","sequence":"first","affiliation":[{"name":"Univ. 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