The electrochemical synthesis of three distinct compounds obtained by the intercalation of hydrated hexilaminium cations [CH3(CH2)(5)NH3+] into the layered compound 2H-NbS2 is reported. They were obtained by cyclovoltammetric and galvanostatic techniques and characterized by x-ray diffractometry. Schematic representations showing the steric arrangement of the hydrated hexilaminium cations in the van der Waals gaps are proposed.