CC BY 3.0 UnportedBresien, JonasFaust, KirillHering-Junghans, ChristianRothe, JuliaSchulz, AxelVillinger, Alexander2022-05-052022-05-052015https://oa.tib.eu/renate/handle/123456789/8865https://doi.org/10.34657/7903Different reactions of Mes* substituted phosphanes (Mes* = 2,4,6-tri-tert-butylphenyl) led to the formation of the bicyclic tetraphosphane Mes*P4Mes* (5) and its unknown Lewis acid adduct 5·GaCl3. In this context, the endo–exo isomer of 5 was fully characterized for the first time. The synthesis was achieved by reactions involving “self-assembly” of the P4 scaffold from P1 building blocks (i.e. primary phosphanes) or by reactions starting from P2 or P4 scaffolds (i.e. a diphosphene or cyclic tetraphosphane). Furthermore, interconversion between the exo–exo and endo–exo isomer were studied by 31P NMR spectroscopy. All compounds were fully characterized by experimental as well as computational methods.enghttps://creativecommons.org/licenses/by/3.0/540Nuclear magnetic resonance spectroscopyScaffoldsSelf assemblyBuilding blockesDiphosphenesInterconversionsLewis AcidPhosphanesSynthetic strategiesIsomersArticle