Synthese und Charakterisierung von Gallium‐Phosphor‐Heterocubanen

Synthesis and Characterization of Gallium‐Phosphorus Heterocubanes The reaction of i PrGaCl 2 with t BuPLi 2 in Et 2 O at −78°C gives the heterocubane [ i PrGaP( t Bu)] 4 ( 1 ) by using the “dilution principle”. {(MesGa) 3 [GaP(H) t Bu][P( t Bu)] 4 } ( 2 ) was formed, when three equivalents of MesGaCl 2 and one equivalent of GaCl 3 in THF at −78°C were treated with 5 equivalents of t BuPLi 2 . Compounds 1 and 2 were characterized by NMR, IR, and MS techniques as well as by X‐ray structure determination. The heterocubane molecules of 1 are disordered in the crystal; every atom site of the central cubical frame work is occupied by gallium and phosphorus atoms (occupation factor 0.5). The structure of 2 contains two crystallographically unique molecules, which are not disordered because of the additional P(H) t Bu groups.