Raman spectroscopy was used to study the complexation in saturated ZnBr2(CdBr2)-CH3CN-H2O solutions at 25-degrees-C within the CN stretching region. Using the Fourier deconvolution procedure for spectral contours, the formation of the complex (CH3CN)Zn2+ in saturated and unsaturated (0.2 mole fraction CH3CN) solutions of the system ZnBr2-CH3CN-H2O was studied. The Fermi resonance interaction between 2253 and 2290 cm-1 determines opposite directions of the combination band shift for the two systems. The differences in complexation of Zn2+ and Cd2+ in the mixed solvent are discussed on the basis of the preferred cation solvation by the solvent molecules.