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Treatment of trans-[MoCl 4 (MeCN) 2 ] with L (L = Me 2 S, Me 2 Se, THT, ½MeSCH 2 CH 2 SMe) in CH 2 Cl 2 solution, or reaction of MoCl 5 with excess L' (L' = n Bu 2 S, n Bu 2 Se, ½MeSCH 2 CH 2 SMe, ½ i PrSCH 2 CH 2 S i Pr, ½MeSCH 2 CH 2 CH 2 SMe, ½MeSeCH 2 CH 2 CH 2 SeMe) in MeCN, produces the Mo(iv) complexes, [MoCl 4 (L) 2 ] and [MoCl 4 (L') 2 ], respectively, in good yield. The new complexes have been characterised by IR and UV-vis spectroscopy, elemental analysis and magnetic measurements, whilst crystal structure analyses of trans-[MoCl 4 (Me 2 S) 2 ], cis-[MoCl 4 {RS(CH 2 ) 2 SR}] (R = Me, i Pr) and cis-[MoCl 4 {MeS(CH 2 ) 3 SMe}] confirmed their identities and distorted octahedral geometries. The potential of [MoCl 4 ( n Bu 2 E) 2 ] (E = S, Se) as the first examples of molybdenum halide derived single source CVD precursors for the growth of MoE 2 thin films was first probed by TGA, which showed multi-step decomposition processes, with the masses of the final residues consistent with MoSe 2 (E = Se) and MoCl 4 (E = S), respectively. Low pressure CVD experiments conducted at 750 °C (E = S) and 525 °C (E = Se) gave silvery and golden yellow films, respectively. Grazing incidence and in plane XRD data confirmed these to be 2H-MoE 2 , whilst the texture of the MoSe 2 was investigated using pole figure measurements. SEM and EDX data, optical and Raman data on the films are also reported.

dalton transactions

Synthesis and properties of MoCl4complexes with thio- and seleno-ethers and their use for chemical vapour deposition of MoSe2and MoS2films