Low-temperature, high yield synthesis, and convenient isolation of the high-electron-density cluster compound Ta6Br14.8H2O for use in biomacromolecular crystallographic phase determination

Low-temperature, high yield synthesis, and convenient isolation of the high-electron-density cluster compound Ta6Br14.8H2O for use in biomacromolecular crystallographic phase determination

Reduction of TaBr(5) with Ga in the presence of KBr in a sealed borosilicate ampule at 400 degrees, followed by aqueous Soxhlet extraction and addition of stannous bromide and hydrobromic acid to the extract, yielded Ta(6)Br(14).8H(2)O in 80-84% yield. The new procedure provides a convenient, low te...

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Veröffentlicht in:Journal of structural biology 2002-09, Vol.139 (3), p.147-151
Hauptverfasser: Hay, Daniel N T, Messerle, Louis
Format: Artikel
Sprache:eng
Schlagworte:
Crystallography, X-Ray - methods
Macromolecular Substances
Organometallic Compounds - chemical synthesis
Organometallic Compounds - chemistry
Temperature
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Zusammenfassung:Reduction of TaBr(5) with Ga in the presence of KBr in a sealed borosilicate ampule at 400 degrees, followed by aqueous Soxhlet extraction and addition of stannous bromide and hydrobromic acid to the extract, yielded Ta(6)Br(14).8H(2)O in 80-84% yield. The new procedure provides a convenient, low temperature, high yield route to the synthesis of the title compound from inexpensive precursors.
ISSN:1047-8477