SYNTHESIS AND CHARACTERIZATION OF GALLIUM-PHOSPHORUS HETEROCUBANES

The reaction of iPrGaCl(2) with tBuPLi(2) in Et(2)O at -78 degrees C gives the heterocubane [iPrGaP(tBu)]4 (1) by using the ''dilution principle''. {(MesGa)(3)[GaP(H)tBu][P(tBu)](4)} (2) was formed, when three equivalents of MesGaCl(2) and one equivalent of GaCl3, in THF at -78 degrees C were treated with 5 equivalents of tBuPLi(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 a 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)tBu groups.