Synthesis and characterization of Mo and W compounds containing aminothiolate ligand for disulfide materials

Mo(VI) and W(VI) compounds containing tBu-imido/aminothiolate ligands, Mo(NtBu)2Cl(dmampS) (1) and W(NtBu)2Cl(dmampS) (4) were prepared through the metathesis reaction of Mo(NtBu)2Cl2(DME) and W(NtBu)2Cl2(py)2 with 1 equiv. of Li(dmampS), and further reaction of 1 and 4 with 1 equiv. of Na(StBu) afforded Mo(NtBu)2(StBu)(dmampS) (3) and W(NtBu)2(StBu)(dmampS) (6), respectively. Mo(NtBu)2(dmampS)2 (2) and W(NtBu)2(dmampS)2 (5) were also synthesized by the reaction of Mo(NtBu)2Cl2(DME) and W(NtBu)2Cl2(py)2 with 2 equiv. Li(dmampS), respectively. Compounds 1–6 were characterized by IR, MS, 1H and 13C NMR spectroscopies, and microanalyses. The molecular structures of 2, 3, 5, and 6 reveal distorted trigonal bipyramidal geometry. Thermogravimetric analyses suggest that residues of 2, 3, 5, and 6 should be MoS2 (2 and 3) and WS2 (5 and 6).

Mo(VI) and W(VI) tBu-imido/aminothiolate compounds 1–6 for molybdenum and tungsten based sulfide thin films were prepared and characterized. Structures of 2, 3, 5, and 6 are distorted trigonal bipyramidal geometry, and the residues of 2, 3, 5, and 6 suggest MoS2 (2 and 3) and WS2 (5 and 6) in TGA. Compounds 3, 4, and 6 are possible to vaporize, especially compound 3 is well vaporized (sublimed at 65 °C/10−1 Torr).Figure optionsDownload as PowerPoint slide