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 temperature, high yield route to the synthesis of the title compound from inexpensive precursors.
Hay
Daniel N T
DN
Department of Chemistry, The University of Iowa, 461 Chemistry Building, Iowa City, IA 52242, USA.
Messerle
Louis
L
D018360:Crystallography, X-Ray / Q000379:methods*; D046911:Macromolecular Substances; D009942:Organometallic Compounds / Q000138:chemical synthesis* / Q000737:chemistry*; D013696:Temperature
D046911:Macromolecular Substances; D009942:Organometallic Compounds