Thermal Decomposition of (NH4)2[Mo3S(S2)6] · nH2O

The thermal decomposition of (NH4)2[Mo3S(S2)6] · nH2O was studied by DTA/TG, infrared spectroscopy, X‐ray diffraction, determination of specific surfaces and temperature programmed desorption measurements. The results are reported and discussed with respect to the stability of the MoIV‐triangle system which is retained during the thermal treatment up to the formation of hexagonal MoS2, which can be understood nicely from a mechanistic point of view.