We report on the intercalation of meso-5, 5, 7, 12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-1,8-diacetate complexed with Co (III) into layered molybdenum disulfide. This is achieved by using the exfoliation and re-stacking properties of LiMoS2. The cobalt complex dissolves readily in a water/acetone solvent mixture. Addition of this solution to an aqueous suspension of single MoS2 layers results in the entrapment of the cobalt macrocycle between the sheets of MoS2. The resulting intercalate was characterized by powder X-ray diffraction and thermogravimetric analysis. (C) 2010 Elsevier B.V. All rights reserved.