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NbSCl 3 was obtained via reaction of NbCl 5 with S(SiMe 3 ) 2 in anhydrous CH 2 Cl 2 , whilst in MeCN solution the same reaction gives [NbSCl 3 (MeCN) 2 ]. [NbSeCl 3 (MeCN) 2 ] was obtained similarly from NbCl 5 with Se(SiMe 3 ) 2 . The chalcogenoether complexes, [NbSCl 3 (ER 2 )] (E = S: R = Me, n Bu; E = Se: R = n Bu), were obtained from reaction of NbCl 5 , ER 2 and S(SiMe 3 ) 2 in CH 2 Cl 2 . The structure of the [Nb 2 S 2 Cl 6 (SMe 2 ) 2 ] reveals a Cl-bridged dimer with the SMe 2 ligands disposed syn. The Cl bridges are highly asymmetric, with the long Nb-Cl bond trans Nb[double bond, length as m-dash]S. The complexes, [NbSCl 3 (L-L)] (L-L = MeSCH 2 CH 2 SMe, MeS(CH 2 ) 3 SMe, i PrSCH 2 CH 2 S i Pr, MeSe(CH 2 ) 3 SeMe and n BuS(CH 2 ) 3 S n Bu), were obtained from reaction of L-L with preformed [NbSCl 3 (MeCN) 2 ]. The structures of the Me-substituted complexes reveal distorted octahedral monomers with the neutral ligands trans to S/Cl. Solution 1 H and 77 Se{ 1 H} NMR data showed that the neutral ligands are partially dissociated and undergoing fast exchange at ambient temperatures in CH 2 Cl 2 solution, consistent with weak Lewis acidity for NbSCl 3 . The complexes containing n Bu-substituted ligands have been used as single source precursors for low pressure chemical vapour deposition (CVD) of 3R-NbS 2 thin films. 2H-NbSe 2 thin films were also obtained via low pressure CVD using [NbSe 2 Cl 3 (Se n Bu 2 )]. The thin films were characterised by grazing incidence and in-plane XRD, pole figure analysis, scanning electron microscopy and energy dispersive X-ray analysis.

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Chalcogenoether complexes of Nb(<scp>v</scp>) thio- and seleno-halides as single source precursors for low pressure chemical vapour deposition of NbS<sub>2</sub> and NbSe<sub>2</sub> thin films

Chalcogenoether complexes of Nb(v) thio- and seleno-halides as single source precursors for low pressure chemical vapour deposition of NbS2 and NbSe2 thin films

Chalcogenoether complexes of Nb(v) thio- and seleno-halides as single source precursors for low pressure chemical vapour deposition of NbS₂ and NbSe₂ thin films