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Stable, preformed nanoclusters, with ligand shells that can undergo additional coordination\u2010driven reactions, provide a platform for assembling multi\u2010cluster solids with precision. Herein, a discrete Co<jats:sub>6<\/jats:sub>S<jats:sub>8<\/jats:sub>(PTA)<jats:sub>6<\/jats:sub> (PTA=1,3,5\u2010triaza\u20107\u2010phosphaadamantane) superatomic\u2010metalloligand is assembled into a three\u2010dimensional (3D) coordination polymer comprising Cu<jats:sub>4<\/jats:sub>I<jats:sub>4<\/jats:sub> secondary building units (SBUs). The resulting heterobimetallic framework (<jats:bold>1<\/jats:bold>) contains two distinct cluster constituents and bifunctional PTA linkers. Solid\u2010state diffuse reflectance studies reveal that <jats:bold>1<\/jats:bold> is an optical semiconductor with a band\u2010gap of 1.59\u2005eV. Framework\u2010modified electrodes exhibit reversible redox behavior in the solid state arising from the Co<jats:sub>6<\/jats:sub>S<jats:sub>8<\/jats:sub> superatoms, which remain intact during framework synthesis.<\/jats:p>","DOI":"10.1002\/chem.202001215","type":"journal-article","created":{"date-parts":[[2020,5,22]],"date-time":"2020-05-22T05:17:35Z","timestamp":1590124655000},"page":"12523-12527","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":8,"title":["Stepwise Assembly of an Electroactive Framework from a Co<sub>6<\/sub>S<sub>8<\/sub> Superatomic Metalloligand and Cuprous Iodide Building Units"],"prefix":"10.1002","volume":"26","author":[{"given":"Matthew B.","family":"Freeman","sequence":"first","affiliation":[{"name":"Department of Chemistry The University of North Carolina at Charlotte  Charlotte North Carolina 28223 USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Ozioma 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