Synthesis and Characterization of tert-Butylgallium−Antimony Compounds: X-ray Crystal Structures of t-Bu3Ga·Sb(SiMe3)3, [t-Bu2GaSb(SiMe3)2]2, and t-Bu2GaSb(SiMe3)2Ga(t-Bu)2Cl, the First Example of a Gallium−Antimony Mixed-Bridge Compound

Abstract

The 1:1 mol ratio reaction of t-Bu3Ga with Sb(SiMe3)3 in hexane yields the expected Lewis acid−base adduct t-Bu3Ga·Sb(SiMe3)3 (1). The 1:1 mol ratio dehalosilylation reaction of t-Bu2GaCl with Sb(SiMe3)3 yields the dimeric compound [t-Bu2GaSb(SiMe3)2]2 (2). The mixed-bridge was isolated from both the 2:1 reaction of t-Bu2GaCl with Sb(SiMe3)3 and the 2:1 equilibration of t-Bu2GaCl with 2. These new gallium−antimony compounds have been characterized through multinuclear solution NMR spectroscopy, partial elemental analysis, and single-crystal X-ray structural analysis. In addition, compound 2 was found to produce nanocrystalline GaSb with an approximate average particle size of 9 nm upon thermolysis at 400 °C under vacuum.