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We herein report on the synthesis of novel bis\u2010phosphaketenes, LM(PCO)<jats:sub>2<\/jats:sub> (M=Ga <jats:bold>2\u2009a<\/jats:bold>, In <jats:bold>2\u2009b<\/jats:bold>; L=HC[C(Me)N(Ar)]<jats:sub>2<\/jats:sub>; Ar=2,6\u2010<jats:italic>i\u2010<\/jats:italic>Pr<jats:sub>2<\/jats:sub>C<jats:sub>6<\/jats:sub>H<jats:sub>3<\/jats:sub>) by salt metathesis reactions and their reactions with LGa to metallaphosphenes LGa(OCP)PML (M=Ga <jats:bold>3\u2009a<\/jats:bold>, In <jats:bold>3\u2009b<\/jats:bold>). <jats:bold>3\u2009b<\/jats:bold> represents the first compound with significant In\u2212P \u03c0\u2010bonding contribution as was confirmed by DFT calculations. Compounds <jats:bold>3\u2009a<\/jats:bold> and <jats:bold>3\u2009b<\/jats:bold> selectively activate the N\u2212H and O\u2212H bonds of aniline and phenol at the Ga\u2212P bond and both reactions proceed with a rearrangement of the phosphaethynolate group from Ga\u2212OCP to M\u2212PCO bonding. Compounds <jats:bold>2\u20135<\/jats:bold> are fully characterized by heteronuclear (<jats:sup>1<\/jats:sup>H, <jats:sup>13<\/jats:sup>C{<jats:sup>1<\/jats:sup>H}, <jats:sup>31<\/jats:sup>P{<jats:sup>1<\/jats:sup>H}) NMR and IR spectroscopy, elemental analysis, and single crystal X\u2010ray diffraction (sc\u2010XRD).<\/jats:p>","DOI":"10.1002\/chem.202200444","type":"journal-article","created":{"date-parts":[[2022,2,28]],"date-time":"2022-02-28T14:03:15Z","timestamp":1646056995000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":22,"title":["Bis\u2010Phosphaketenes LM(PCO)<sub>2<\/sub> (M=Ga, In): A New Class of Reactive Group 13 Metal\u2010Phosphorus Compounds"],"prefix":"10.1002","volume":"28","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-3116-6631","authenticated-orcid":false,"given":"Mahendra K.","family":"Sharma","sequence":"first","affiliation":[{"name":"Institute of Inorganic Chemistry University of Duisburg-Essen  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