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Unprecedented functionalized, contracted as well as complexly aggregated polyphosphorus compounds are accessed utilizing [Cp*Fe(\u03b7<jats:sup>5<\/jats:sup>\u2010P<jats:sub>5<\/jats:sub>Me)][OTf] (<jats:bold>A<\/jats:bold>), highlighting the great potential of this underexplored mode of reactivity. Addition of carbenes to <jats:bold>A<\/jats:bold> affords novel 1,2\u2010 or 1,1\u2010difunctionalized cyclo\u2010P<jats:sub>5<\/jats:sub> complexes [Cp*Fe(\u03b7<jats:sup>4<\/jats:sup>\u2010P<jats:sub>5<\/jats:sub>(1\u2010L)(2\u2010Me)][OTf] (L=IDipp (<jats:bold>1<\/jats:bold>), <jats:sup>Et<\/jats:sup>CAAC (<jats:bold>2<\/jats:bold>), I<jats:sup>i<\/jats:sup>Pr (<jats:bold>3\u2009b<\/jats:bold>)) and [Cp*Fe(\u03b7<jats:sup>4<\/jats:sup>\u2010P<jats:sub>5<\/jats:sub>(1\u2010I<jats:sup>i<\/jats:sup>Pr)(1\u2010Me)][OTf] (<jats:bold>3\u2009a<\/jats:bold>). For the first time, the much smaller IMe<jats:sub>4<\/jats:sub> leads to the contraction of the cyclo\u2010P<jats:sub>5<\/jats:sub> ligand and formation of [Cp*Fe(\u03b7<jats:sup>4<\/jats:sup>\u2010P<jats:sub>4<\/jats:sub>(1\u2010IMe)(4\u2010Me)] (<jats:bold>4<\/jats:bold>). DFT calculations shed light on the delicate mechanism of this type of reaction, which is reinforced by the experimental identification of key intermediates. Even the comparably weak nucleophile IDippCH<jats:sub>2<\/jats:sub> reacts with <jats:bold>A<\/jats:bold> to form [Cp*Fe(\u03b7<jats:sup>4<\/jats:sup>\u2010P<jats:sub>5<\/jats:sub>(1\u2010IDippCH<jats:sub>2<\/jats:sub>)(1\/2\u2010Me)][OTf] (<jats:bold>6\u2009a<\/jats:bold>\/<jats:bold>b<\/jats:bold>), highlighting its explicitly more reactive nature. Moreover, exposure of <jats:bold>A<\/jats:bold> to IDippEH (E=N, P) leads to a unique aggregation reaction affording [{Cp*Fe}<jats:sub>2<\/jats:sub>{\u03bc<jats:sub>2<\/jats:sub>,\u03b7<jats:sup>4:3:1<\/jats:sup>\u2013P<jats:sub>10<\/jats:sub>Me<jats:sub>2<\/jats:sub>(IDippN)}][OTf] (<jats:bold>8<\/jats:bold>) and [{Cp*Fe}<jats:sub>2<\/jats:sub>{\u03bc<jats:sub>2<\/jats:sub>,\u03b7<jats:sup>4:1:1:1<\/jats:sup>\u2013P<jats:sub>11<\/jats:sub>Me<jats:sub>2<\/jats:sub>(IDipp)}][OTf] (<jats:bold>9<\/jats:bold>), respectively.<\/jats:p>","DOI":"10.1002\/chem.202402675","type":"journal-article","created":{"date-parts":[[2024,9,30]],"date-time":"2024-09-30T06:30:03Z","timestamp":1727677803000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["Enhancing the Reactivity of an Aromatic <i>cyclo<\/i>\u2010P<sub>5<\/sub> Ligand via Electrophilic Activation"],"prefix":"10.1002","volume":"30","author":[{"ORCID":"https:\/\/orcid.org\/0009-0003-3590-9919","authenticated-orcid":false,"given":"Christoph","family":"Riesinger","sequence":"first","affiliation":[{"name":"Institute of Inorganic Chemistry University of Regensburg  Regensburg 93040 Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Philip M.","family":"Blank","sequence":"additional","affiliation":[{"name":"Laboratory of Organic Chemistry ETH Z\u00fcrich  Vladimir-Prelog-Weg 3, HCI Z\u00fcrich 8093 Switzerland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Christian","family":"Scholtes","sequence":"additional","affiliation":[{"name":"Institute of Organic Chemistry University of Regensburg  Regensburg 93040 Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ruth M.","family":"Gschwind","sequence":"additional","affiliation":[{"name":"Institute of Organic Chemistry University of Regensburg  Regensburg 93040 Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2182-5020","authenticated-orcid":false,"given":"Manfred","family":"Scheer","sequence":"additional","affiliation":[{"name":"Institute of Inorganic Chemistry University of Regensburg  Regensburg 93040 Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2024,11,7]]},"reference":[{"key":"e_1_2_8_1_1","doi-asserted-by":"crossref","first-page":"204","DOI":"10.1007\/BF01339530","volume":"70","author":"H\u00fcckel E.","year":"1931","journal-title":"Z. 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