Abstract
The treatment of (TBA)TcO4 with conc. HCl or HBr at room temperature yields (TBA)[TcOCl4] or (TBA)[TcOBr4], which are nearly insoluble in acidic aqueous solutions, but well soluble in organic solvents. The vibrational spectra indicate C4v symmetry for the complex ions. (TBA)[TcOBr4] shows an unusual resonance Raman effect, as the progression of overtones runs with the B1 TcCL4 stretching vibration instead of the symmetric A1 mode. The coupling of B1 with the first overtone of νTcO gives more intense difference than combination bands.