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In this study, we introduce a new [3+1] fragmentation procedure for <jats:italic>cyclo<\/jats:italic>\u2010P<jats:sub>4<\/jats:sub> ligands, leading to the discovery of acylcyanophosphanides and \u2010phosphines. Treatment of the complex [K(18c\u20106)][(Ar*BIAN)Co(\u03b7<jats:sup>4<\/jats:sup>\u2010P<jats:sub>4<\/jats:sub>)] ([K(18c\u20106)]<jats:bold>3<\/jats:bold>, 18c\u20106=[18]crown\u20106, Ar*=2,6\u2010dibenzhydryl\u20104\u2010isopropylphenyl, BIAN=1,2\u2010bis(arylimino)acenaphthene diimine) with acyl chlorides results in the formation of acylated tetraphosphido complexes [(Ar*BIAN)Co(\u03b7<jats:sup>4<\/jats:sup>\u2010P<jats:sub>4<\/jats:sub>C(O)R)] (R=<jats:italic>t<\/jats:italic>Bu, Cy, 1\u2010Ad, Ph; <jats:bold>4\u2009a<\/jats:bold>\u2013<jats:bold>d<\/jats:bold>). Subsequent reactions of <jats:bold>4\u2009a<\/jats:bold>\u2013<jats:bold>d<\/jats:bold> with cyanide salts yield acylated cyanophosphanides [RC(O)PCN]<jats:sup>\u2212<\/jats:sup> (<jats:bold>9\u2009a<\/jats:bold>\u2013<jats:bold>d<\/jats:bold><jats:sup>\u2212<\/jats:sup>) and the <jats:italic>cyclo<\/jats:italic>\u2010P<jats:sub>3<\/jats:sub> cobaltate anion [(Ar*BIAN)Co(\u03b7<jats:sup>3<\/jats:sup>\u2010P<jats:sub>3<\/jats:sub>)(CN)]<jats:sup>\u2212<\/jats:sup> (<jats:bold>8<\/jats:bold><jats:sup>\u2212<\/jats:sup>). Further reactions of <jats:bold>4\u2009a<\/jats:bold>\u2013<jats:bold>d<\/jats:bold> with trimethylsilyl cyanide (Me<jats:sub>3<\/jats:sub>SiCN) and isocyanides provide insight into a plausible mechanism of this [3+1] fragmentation reaction, as these reagents partially displace the P<jats:sub>4<\/jats:sub>C(O)R ligand from the cobalt center. Several potential intermediates of the [3+1] fragmentation were characterized. Additionally, the introduction of a second acyl substituent was achieved by treating [K(18c\u20106)]<jats:bold>9b<\/jats:bold> with CyC(O)Cl, resulting in the first bis(acyl)monocyanophosphine (CyC(O))<jats:sub>2<\/jats:sub>PCN (<jats:bold>10<\/jats:bold>).<\/jats:p>","DOI":"10.1002\/anie.202317170","type":"journal-article","created":{"date-parts":[[2023,12,8]],"date-time":"2023-12-08T02:08:32Z","timestamp":1702001312000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":14,"title":["Cobalt\u2010Mediated [3+1] Fragmentation of White Phosphorus: Access to Acylcyanophosphanides"],"prefix":"10.1002","volume":"63","author":[{"ORCID":"https:\/\/orcid.org\/0009-0009-9963-4751","authenticated-orcid":false,"given":"Sebastian","family":"Hauer","sequence":"first","affiliation":[{"name":"University of Regensburg Institute of Inorganic Chemistry  93040 Regensburg Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5027-450X","authenticated-orcid":false,"given":"Thomas M.","family":"Horsley Downie","sequence":"additional","affiliation":[{"name":"University of Regensburg Institute of Inorganic Chemistry  93040 Regensburg Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3497-7082","authenticated-orcid":false,"given":"G\u00e1bor","family":"Bal\u00e1zs","sequence":"additional","affiliation":[{"name":"University of Regensburg Institute of Inorganic Chemistry  93040 Regensburg Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7965-2647","authenticated-orcid":false,"given":"Kai","family":"Schwedtmann","sequence":"additional","affiliation":[{"name":"TU Dresden Faculty of Chemistry and Food Chemistry  01062 Dresden Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7323-7816","authenticated-orcid":false,"given":"Jan J.","family":"Weigand","sequence":"additional","affiliation":[{"name":"TU Dresden Faculty of Chemistry and Food Chemistry  01062 Dresden Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4066-6483","authenticated-orcid":false,"given":"Robert","family":"Wolf","sequence":"additional","affiliation":[{"name":"University of Regensburg Institute of Inorganic Chemistry  93040 Regensburg Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2024,1,2]]},"reference":[{"key":"e_1_2_7_1_1","unstructured":"Selected literature for the synthesis of phosphorus compounds:"},{"key":"e_1_2_7_2_2","volume-title":"Phosphorus 2000. 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