The reaction of methane with sulfur at 973 K and an S-2 : CH4 ratio of 1.4 in the presence of Al2O3-supported mono- or bimetallic molybdenum and nickel sulfide catalysts was studied. The Mo-Ni sulfide catalyst pretreated with methane at 973 K had a high activity in the formation of hydrocarbons. The main hydrocarbon products were cyclopentane and aliphatic C-5 hydrocarbons. Cyclopentane yielded aliphatic C-5 hydrocarbons with an increasing nickel content in Mo-Ni sulfide.