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The diamagnetic mononuclear complexes [Ni(L)] show a distorted square\u2010planar N<jats:sub>2<\/jats:sub>S<jats:sub>2<\/jats:sub> coordination environment and have been characterized by <jats:sup>1<\/jats:sup>H\u2010 and <jats:sup>13<\/jats:sup>C\u2005NMR and UV\/Vis spectroscopies and by single\u2010crystal X\u2010ray crystallography. Cyclic voltammetry and coulombic measurements have established that complexes <jats:bold>1<\/jats:bold> and <jats:bold>2<\/jats:bold>, incorporating <jats:italic>t<\/jats:italic>Bu functionalities on the thiophenolate ligands, undergo reversible one\u2010electron oxidation processes, whereas the analogous redox processes for complexes <jats:bold>3<\/jats:bold> and <jats:bold>4<\/jats:bold> are not reversible. The one\u2010electron oxidized species, <jats:bold>1<jats:sup>+<\/jats:sup><\/jats:bold> and <jats:bold>2<jats:sup>+<\/jats:sup><\/jats:bold>, can be generated quantitatively either electrochemically or chemically with 70\u2009% HClO<jats:sub>4<\/jats:sub>. EPR and UV\/Vis spectroscopic studies and supporting DFT calculations suggest that the SOMOs of <jats:bold>1<\/jats:bold><jats:sup>+<\/jats:sup> and <jats:bold>2<\/jats:bold><jats:sup>+<\/jats:sup> possess thiyl radical character, whereas those of <jats:bold>1<\/jats:bold>(py)<jats:sub>2<\/jats:sub><jats:sup>+<\/jats:sup> and <jats:bold>2<\/jats:bold>(py)<jats:sub>2<\/jats:sub><jats:sup>+<\/jats:sup> possess formal Ni<jats:sup>III<\/jats:sup> centers. Species <jats:bold>2<jats:sup>+<\/jats:sup><\/jats:bold> dimerizes at low temperature, and an X\u2010ray crystallographic determination of the dimer [(<jats:bold>2<\/jats:bold>)<jats:sub>2<\/jats:sub>](ClO<jats:sub>4<\/jats:sub>)<jats:sub>2<\/jats:sub>\u22c52\u2009CH<jats:sub>2<\/jats:sub>Cl<jats:sub>2<\/jats:sub> confirms that this dimerization involves the formation of a S\uf8ffS bond (S\u22c5\u22c5\u22c5S=2.202(5)\u2005\u00c5).<\/jats:p>","DOI":"10.1002\/chem.200701108","type":"journal-article","created":{"date-parts":[[2008,1,21]],"date-time":"2008-01-21T13:28:13Z","timestamp":1200922093000},"page":"2564-2576","source":"Crossref","is-referenced-by-count":47,"title":["Molecular and Electronic Structures of One\u2010Electron Oxidized Ni<sup>II<\/sup>\u2013(Dithiosalicylidenediamine) Complexes: Ni<sup>III<\/sup>\u2013Thiolate versus Ni<sup>II<\/sup>\u2013Thiyl Radical States"],"prefix":"10.1002","volume":"14","author":[{"given":"Philip\u2005A.","family":"Stenson","sequence":"first","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Ashley","family":"Board","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Armando","family":"Marin\u2010Becerra","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Alexander\u2005J.","family":"Blake","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"E.\u2005Stephen","family":"Davies","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Claire","family":"Wilson","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Jonathan","family":"McMaster","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Martin","family":"Schr\u00f6der","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"311","published-online":{"date-parts":[[2008,2,28]]},"reference":[{"key":"e_1_2_6_1_2","unstructured":"\u00a0"},{"key":"e_1_2_6_2_2","doi-asserted-by":"publisher","DOI":"10.1016\/S0969-2126(97)00313-4"},{"key":"e_1_2_6_3_2","doi-asserted-by":"publisher","DOI":"10.1016\/S0969-2126(99)80071-9"},{"key":"e_1_2_6_4_2","first-page":"1055","volume":"219","author":"Spencer D. 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