Abstract:Well oriented KYb(WO 4 ) 2 and KTb 0 2 Yb 0 8 (WO 4 ) 2 single crystals have been investigated for their magnetic and optical properties using the Raman and EPR techniques. The registered EPR signal is dominated by three lines ascribed to ytterbium ions: one main and two satellites. Tb ions, although non-paramagnetic, distinctly modify magnetic properties of the KYb(WO 4 ) 2 single crystal. Basic parameters of the spin Hamiltonian, including Zeeman and hyperfine terms (g and A matrices) as well the spatial orientation between principal and crystallographic axes systems were determined for both crystals.