AgSnBiSe3 and AgSnBiSe2S were prepared by solid state reactions at 950 °C. The phases were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), and Raman spectroscopy. The samples were indexed in two space groups: Pm3̅m (No. 221) and P4/mmm (No. 123). The Raman spectra confirmed the structure of the AgSnBiSe3 and AgSnBiSe2S compounds to be distorted NaCl-type with seven characteristic signals for the Raman active modes.