The synthesis, characterization and crystal structure of (NH4)AgMoS4 is presented. (NH4)AgMoS4 was prepared by the stoichiometric reaction of AgNO3 with (NH4)2MoS4. The black microcrystalline (NH4)AgMoS4 is thermally unstable and contaminated by a phase that analyzes for Ag2MoS4. In the TGA continuous weight loss was observed corresponding to the loss of ammonia gas subsequent loss of sulfur and H2S to give Ag2S and MoS2. In the infrared spectrum of (NH4)AgMoS4, characteristic bands for the ammonium ion at 1350–1400 cm–1 and for the [MoS4]2– group at 460 cm–1 are observed. Crystals of (NH4)AgMoS4 were investigated using a synchroton source. (NH4)AgMoS4 is isostructural to (NH4)CuMoS4 and crystallizes in the tetragonal space group I$\bar{4}$ (Z = 2, a = 7.8740(3), c = 5.7733(4) Å). (NH4)AgMoS4 can be used as a catalyst in the syngas conversion to higher alcohols with showing good activity and ethanol selectivity.