Accession Number : ADA328875

Title :   Synthesis and Characterization of Tert-Butylgallium-Antimony Compounds; X-Ray Crystal Structures of t-Bu3Ga. Sb(SiMe3)3, T-Bu2GaSb(SiMe3)2, and t-Bu2GaSb(SiMe3)Ga(t-Bu)2Cl, The first Example of a Gallium-Antimony Mixed-Bridge Compound

Descriptive Note : Technical rept.

Corporate Author : DUKE UNIV DURHAM NC DEPT OF CHEMISTRY

Personal Author(s) : Wells, Richard L. ; Foos, Edward E. ; White, Peter S. ; Rheingold, Arnold L. ; Liable-Sands, Louise M.

PDF Url : ADA328875

Report Date : 30 AUG 1997

Pagination or Media Count : 25

Abstract : The 1:1 mole 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 mole ratio dehalosilylation reaction of t-Bu2GaCl with Sb(SiMe3)3 yields the dimeric compound T-Bu2GaSb(SiMe3)22) (2). The mixed-bridge compound t-Bu2GaSb(SiMe3)3Ga(t-Bu)2Cl (3) 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 deg C under vacuum.

Descriptors :   *GALLIUM, *ANTIMONY, CRYSTAL STRUCTURE, NUCLEAR MAGNETIC RESONANCE, SPECTROSCOPY, METHYL RADICALS, SYNTHESIS, STRUCTURAL ANALYSIS, VACUUM, SINGLE CRYSTALS, ORGANOMETALLIC COMPOUNDS, X RAYS, SILICON, CHLORIDES, BUTYL RADICALS, DIMERS, HEXANES.

Subject Categories : Inorganic Chemistry
      Organic Chemistry
      Physical Chemistry
      Crystallography

Distribution Statement : APPROVED FOR PUBLIC RELEASE