The reaction of [MoO2((CH3)HN-O)2] and N-methylhydroxylammoniumchloride in an aqueous suspension with CS2 yields red crystals of the analytical composition MOC4H14N3O4S2. The crystal structure has been determined by single crystal X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P21/c, with cell constants a= 1333.2(3), b = 814.2(2), c = 2179.8(6) pm, β = 105.42(2)°, and Z = 8. The final R-value is 4.5% for 2965 unique reflexions. The structure consists of two crystallographically independent neutral complexes of molybdenum(VI). The geometry about the molybdenum is a distorted pentagonal bipyramid containing a terminal oxygen atom, two N-methylhydroxylamido(1-) ligands coordinated via the O-and N-atoms and an N-methyl-N-oxo-dithiocarbamato(2-) ligand forming a planar five membered ring with the molybdenum(VI) center (O,S-coordination).