A series of intercalation compounds of tetraazamacrocycles in molybdenum disulfide have been synthesized using the exfoliation and restacking properties of LiMoS2. The sandwiched compounds were characterized by powder X-ray diffraction, thermogravimetric analyses, differential scanning calorimetry, and four-probe electrical conductivity measurements. The interlayer spacing of the intercalation compound was found to be dependent on the size of the macrocyclic ligand, indicating that the intercalated macrocycles are co-planar with the MoS2 sheets.