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CuII catalyst is less efficient at room temperature for C−S cross‐coupling. C−S cross‐coupling by CuII catalyst at room temperature is not reported; however, doping of copper with molybdenum metal has been realized here to be more efficient for C−S cross‐coupling in comparison to general CuII catalyst. The doped catalyst CuMoO4 nanoparticle is found to be more efficient than copper. The catalyst works under mild conditions without any ligand at room temperature and is recyclable and effective for a wide range of thiols and haloarenes (ArI, ArBr, ArF) from milligram to gram scale. The copper‐based bimetallic catalyst is developed and recognized for C−S cross‐coupling of haloarenes with alkyl and aryl thiols. [ABSTRACT FROM AUTHOR]