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We have reported that the combination of a phosphinidene transfer agent, <jats:sup>Ar<\/jats:sup>TerP(PMe<jats:sub>3<\/jats:sub>) (<jats:sup>Ar<\/jats:sup>Ter=2,6\u2010Ar<jats:sub>2<\/jats:sub>\u2010C<jats:sub>6<\/jats:sub>H<jats:sub>3<\/jats:sub>), with (Cp*Al)<jats:sub>4<\/jats:sub> (Cp*=C<jats:sub>5<\/jats:sub>(CH<jats:sub>3<\/jats:sub>)<jats:sub>5<\/jats:sub>) afforded the phosphaalumenes <jats:sup>Ar<\/jats:sup>TerPAlCp* as isolable, violet, thermally stable compounds. In here we describe attempts to utilize Mes*P(PMe<jats:sub>3<\/jats:sub>) (Mes*=2,4,6\u2010<jats:italic>t<\/jats:italic>Bu<jats:sub>3<\/jats:sub>\u2010C<jats:sub>6<\/jats:sub>H<jats:sub>2<\/jats:sub>) as a phosphinidene source in combination with different Al(I) precursors, namely <jats:sup>Dip<\/jats:sup>NacnacAl (<jats:sup>Dip<\/jats:sup>Nacnac=HC[C(Me)NDip]<jats:sub>2<\/jats:sub>, Dip=2,6\u2010<jats:italic>i<\/jats:italic>Pr<jats:sub>2<\/jats:sub>\u2010C<jats:sub>6<\/jats:sub>H<jats:sub>3<\/jats:sub>), (Cp*Al)<jats:sub>4<\/jats:sub> and Cp<jats:sup>3t<\/jats:sup>Al (Cp<jats:sup>3t<\/jats:sup>=1,2,4\u2010<jats:italic>t<\/jats:italic>Bu<jats:sub>3<\/jats:sub>\u2010C<jats:sub>5<\/jats:sub>H<jats:sub>2<\/jats:sub>). In all cases the formation of phosphaalumenes was not observed, however, their intermediate formation is indicated by formation of the dimer [Cp*Al(\u03bc\u2010PMes*)]<jats:sub>2<\/jats:sub> (<jats:bold>2<\/jats:bold>) and C\u2212H\u2010bond activation products along the putative P=Al bond, giving unusual 1,2\u2010P,Al\u2010tetrahydronaphtalene derivatives <jats:bold>1<\/jats:bold> and <jats:bold>4<\/jats:bold>, clearly underlining the role the sterically demanding group on phosphorus plays in these transformations. The reactivity studies are supported by theoretical studies, demonstrating a thermodynamic preference for the C\u2212H activation products. Additionally, we show that there are potential pitfalls in the synthesis of Cp*<jats:sub>2<\/jats:sub>AlH, the precursor to make (Cp*Al)<jats:sub>4<\/jats:sub> and give recommendations how to circumvent these.<\/jats:p>","DOI":"10.1002\/cplu.202300078","type":"journal-article","created":{"date-parts":[[2023,2,24]],"date-time":"2023-02-24T01:56:04Z","timestamp":1677203764000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":13,"title":["On the Reactivity of Mes*P(PMe<sub>3<\/sub>) towards Aluminum(I) Compounds \u2013 Evidence for the Intermediate Formation of Phosphaalumenes"],"prefix":"10.1002","volume":"88","author":[{"given":"Samuel","family":"Nees","sequence":"first","affiliation":[{"name":"Institut f\u00fcr Anorganische Chemie Julius-Maximilians-Universit\u00e4t W\u00fcrzburg  Am Hubland 97074 W\u00fcrzburg Germany"},{"name":"Institute for Sustainable Chemistry &amp; Catalysis with Boron Julius-Maximilians-Universit\u00e4t W\u00fcrzburg  Am Hubland 97074 W\u00fcrzburg Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4430-982X","authenticated-orcid":false,"given":"Henrik","family":"Beer","sequence":"additional","affiliation":[{"name":"Leibniz-Institut f\u00fcr Katalyse e.V. 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