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The new oxo\u2010alkoxide compounds were fully characterized by spectroscopic methods, magnetic susceptibility measurement, DFT and ab initio computational methods, and complete single\u2010crystal X\u2010ray diffraction structure analysis. The isostructural clusters are formed of edge\u2010sharing octahedral {VO<jats:sub>5<\/jats:sub>N} and trigonal bipyramidal {MO<jats:sub>3<\/jats:sub>NCl} units. Diethanolamine ligates the bimetallic lacunary double cubane core of <jats:bold>1<\/jats:bold> and <jats:bold>2<\/jats:bold> in an unusual two\u2010mode fashion, unobserved previously. In the crystalline state, the clusters of <jats:bold>1<\/jats:bold> and <jats:bold>2<\/jats:bold> are joined by hydrogen bonds to form a three\u2010dimensional network structure. Magnetic susceptibility data indicate weakly antiferromagnetic interactions between the vanadium centers [<jats:italic>J<\/jats:italic><jats:sub>iso<\/jats:sub>(V<jats:sup>IV<\/jats:sup>\u2212V<jats:sup>IV<\/jats:sup>)=\u22125.4(<jats:bold>1<\/jats:bold>); \u22123.9(<jats:bold>2<\/jats:bold>) cm<jats:sup>\u22121<\/jats:sup>], and inequivalent antiferromagnetic interactions between the cobalt and vanadium centers [<jats:italic>J<\/jats:italic><jats:sub>iso<\/jats:sub> (V<jats:sup>IV<\/jats:sup>\u2212Co<jats:sup>II<\/jats:sup>)=\u221212.6 and \u22127.5\u2005cm<jats:sup>\u22121<\/jats:sup>] contained in <jats:bold>1<\/jats:bold>.<\/jats:p>","DOI":"10.1002\/chem.202301389","type":"journal-article","created":{"date-parts":[[2023,7,27]],"date-time":"2023-07-27T12:32:04Z","timestamp":1690461124000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Organo\u2010Functionalized Lacunary Double Cubane\u2010Type Oxometallates: Synthesis, Structure, and Properties of [(M<sup>II<\/sup>Cl)<sub>2<\/sub>(V<sup>IV<\/sup>O)<sub>2<\/sub>{((HOCH<sub>2<\/sub>CH<sub>2<\/sub>)(H)N(CH<sub>2<\/sub>CH<sub>2<\/sub>O))(HN(CH<sub>2<\/sub>CH<sub>2<\/sub>O)<sub>2<\/sub>)}<sub>2<\/sub>] (M=Co, Zn)"],"prefix":"10.1002","volume":"29","author":[{"given":"Damola T.","family":"Shuaib","sequence":"first","affiliation":[{"name":"Department of Chemistry Illinois Institute of Technology  Chicago IL 60616 USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"LaSalle","family":"Swenson","sequence":"additional","affiliation":[{"name":"Department of Chemistry Illinois Institute of Technology  Chicago IL 60616 USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"James A.","family":"Kaduk","sequence":"additional","affiliation":[{"name":"Department of Chemistry Illinois Institute of Technology  Chicago IL 60616 USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Tieyan","family":"Chang","sequence":"additional","affiliation":[{"name":"ChemMatCARS The University of Chicago  Lemont IL 60439 USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Yu\u2010Sheng","family":"Chen","sequence":"additional","affiliation":[{"name":"ChemMatCARS The University of Chicago  Lemont IL 60439 USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"James","family":"McNeely","sequence":"additional","affiliation":[{"name":"Department of Chemistry Boston University  Boston MA 02215 USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8799-5738","authenticated-orcid":false,"given":"M. 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