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The association of <jats:bold>1<\/jats:bold> with in\u2005situ prepared [Fe<jats:sup>II<\/jats:sup>(bik)<jats:sub>2<\/jats:sub>(MeCN)<jats:sub>2<\/jats:sub>](OTf)<jats:sub>2<\/jats:sub> (bik=bis(1\u2010methylimidazol\u20102\u2010yl)ketone) leads to a molecular square of formula {[Co<jats:sup>III<\/jats:sup>{(<jats:sup>Me2<\/jats:sup>Tp)}(CN)<jats:sub>3<\/jats:sub>]<jats:sub>2<\/jats:sub>[Fe<jats:sup>II<\/jats:sup>(bik)<jats:sub>2<\/jats:sub>]<jats:sub>2<\/jats:sub>}(OTf)<jats:sub>2<\/jats:sub>\u2009\u22c5\u20094MeCN\u2009\u22c5\u20092H<jats:sub>2<\/jats:sub>O (<jats:bold>2<\/jats:bold>), whereas the self\u2010assembly of <jats:bold>1<\/jats:bold> with preformed cluster [Co<jats:sup>II<\/jats:sup><jats:sub>2<\/jats:sub>(OH<jats:sub>2<\/jats:sub>)(piv)<jats:sub>4<\/jats:sub>(Hpiv)<jats:sub>4<\/jats:sub>] in MeCN leads to the two\u2010dimensional network of formula {[Co<jats:sup>II<\/jats:sup><jats:sub>2<\/jats:sub>(piv)<jats:sub>3<\/jats:sub>]<jats:sub>2<\/jats:sub>[Co<jats:sup>III<\/jats:sup>(<jats:sup>Me2<\/jats:sup>Tp)(CN)<jats:sub>3<\/jats:sub>]<jats:sub>2<\/jats:sub>\u2009\u22c5\u20092CH<jats:sub>3<\/jats:sub>CN}<jats:sub>\u221e<\/jats:sub> (<jats:bold>3<\/jats:bold>). These compounds were structurally characterized via single crystal X\u2010ray analysis and their spectroscopic (FTIR, UV\u2010Vis and <jats:sup>59<\/jats:sup>Co NMR) properties and magnetic behaviours were also investigated. Bulk magnetic susceptibility measurements reveal that <jats:bold>1<\/jats:bold> is diamagnetic and <jats:bold>3<\/jats:bold> is paramagnetic throughout the explored temperature range, whereas <jats:bold>2<\/jats:bold> exhibits sharp spin transition centered at ca. 292\u2005K. Compound <jats:bold>2<\/jats:bold> also exhibits photomagnetic effects at low temperature, selective light irradiations allowing to promote reversibly and repeatedly low\u2010spin\u21d4high\u2010spin conversion. Besides, the diamagnetic nature of the Co(III) building block allows us studying these compounds by means of <jats:sup>59<\/jats:sup>Co NMR spectroscopy. Herein, a <jats:sup>59<\/jats:sup>Co chemical shift has been used as a magnetic probe to corroborate experimental magnetic data obtained from bulk magnetic susceptibility measurements. An influence of the magnetic state of the neighbouring atoms is observed on the <jats:sup>59<\/jats:sup>Co NMR signals. Moreover, for the very first time, <jats:sup>59<\/jats:sup>Co NMR technique has been successfully introduced to investigate molecular materials with distinct magnetic properties.<\/jats:p>","DOI":"10.1002\/chem.202200783","type":"journal-article","created":{"date-parts":[[2022,6,18]],"date-time":"2022-06-18T05:30:11Z","timestamp":1655530211000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["Molecular Magnetic Materials Based on {Co<sup>III<\/sup>(Tp*)(CN)<sub>3<\/sub>}<sup>\u2212<\/sup> Cyanidometallate: Combined Magnetic, Structural and <sup>59<\/sup>Co NMR Study"],"prefix":"10.1002","volume":"28","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-4976-1113","authenticated-orcid":false,"given":"Siddhartha","family":"De","sequence":"first","affiliation":[{"name":"Institut Parisien de Chimie Mol\u00e9culaire UMR CNRS 8232 Sorbonne Universit\u00e9, CNRS  75005 Paris France"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Alexandrine","family":"Flambard","sequence":"additional","affiliation":[{"name":"Institut Parisien de Chimie Mol\u00e9culaire UMR CNRS 8232 Sorbonne Universit\u00e9, CNRS  75005 Paris France"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Buqin","family":"Xu","sequence":"additional","affiliation":[{"name":"Institut Parisien de Chimie Mol\u00e9culaire UMR CNRS 8232 Sorbonne Universit\u00e9, CNRS  75005 Paris France"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Lise\u2010Marie","family":"Chamoreau","sequence":"additional","affiliation":[{"name":"Institut Parisien de Chimie Mol\u00e9culaire UMR CNRS 8232 Sorbonne Universit\u00e9, CNRS  75005 Paris France"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Geoffrey","family":"Gontard","sequence":"additional","affiliation":[{"name":"Institut Parisien de Chimie Mol\u00e9culaire UMR CNRS 8232 Sorbonne Universit\u00e9, CNRS  75005 Paris France"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8649-9022","authenticated-orcid":false,"given":"Laurent","family":"Lisnard","sequence":"additional","affiliation":[{"name":"Institut Parisien de Chimie Mol\u00e9culaire UMR CNRS 8232 Sorbonne Universit\u00e9, CNRS  75005 Paris France"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9581-7608","authenticated-orcid":false,"given":"Yanling","family":"Li","sequence":"additional","affiliation":[{"name":"Institut Parisien de Chimie Mol\u00e9culaire UMR CNRS 8232 Sorbonne Universit\u00e9, CNRS  75005 Paris France"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6710-4523","authenticated-orcid":false,"given":"Marie\u2010Laure","family":"Boillot","sequence":"additional","affiliation":[{"name":"Institut Chimie Mol\u00e9culaire et Mat\u00e9riaux d'Orsay UMR CNRS 8182 Universit\u00e9 Paris-Saclay, CNRS  91405 Orsay France"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3510-5112","authenticated-orcid":false,"given":"Rodrigue","family":"Lescou\u00ebzec","sequence":"additional","affiliation":[{"name":"Institut Parisien de Chimie Mol\u00e9culaire UMR CNRS 8232 Sorbonne Universit\u00e9, CNRS  75005 Paris France"}],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"311","published-online":{"date-parts":[[2022,7,20]]},"reference":[{"key":"e_1_2_7_1_1","unstructured":"\u00a0"},{"key":"e_1_2_7_2_2","first-page":"155","volume-title":"Cyanide-Bridged Complexes of Transition Metals: A Molecular Magnetism Perspective","author":"Shatruk M.","year":"2009"},{"key":"e_1_2_7_3_2","doi-asserted-by":"publisher","DOI":"10.1126\/science.268.5209.397"},{"key":"e_1_2_7_4_2","first-page":"1","volume-title":"Inorganic Chemistry. 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