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A family of cyclic phosphine‐disiloxane featuring peri‐substituted naphthyl(Nap)/acenaphthyl(Ace) scaffolds has been prepared and fully characterized including X‐ray structure, which enables a detailed structural analysis. This straightforward synthesis takes advantage of both ortho‐ and peri‐substitution of Nap/Ace‐substituted phosphine oxides. The synthetic method allows diversifying the polycyclic aromatic platform (Nap and Ace) as well as the Si substituents (Me and Ph). Despite a strong steric congestion, the P‐atom remains reactive toward oxidation or coordination. In particular, Au(I) complex could be prepared. All the compounds display absorption/luminescence in the UV‐Vis range. Surprisingly, the P‐trivalent derivatives display unexpected luminescence in the green in solid‐state. [ABSTRACT FROM AUTHOR]

In this article, we describe the synthesis of polyaromatic heteropines including main group element (Phosphorus, Germanium) through Ni or Cu‐mediated C−C coupling. Coordination complexes were synthesized with the σ3,λ3‐phosphepines using different metal ions (Au(I), Re(I), Pd(II)) showing that these P‐heterocycles display the classical reactivity of two‐electrons P‐donor making them promising ligands. The optical properties were experimentally studied (UV‐vis absorption and emission) and compared. Finally, both polyaromatic germepine and phosphepine appear as interesting building blocks for optoelectronics. [ABSTRACT FROM AUTHOR]