Synthesis and crystal structure of tris(diethyldithiocarbamato-S,S′)(disulfido-S,S′)niobium(V)
Abstract
The reaction of [NbVO(S2CNEt2)3] with boron sulfide was investigated under a variety of conditions. The major product in all cases was yellow [NbVS(S2CNEt2)3]1. In dichloromethane at room temperature, orange [NbV(S2)(S2CNEt2)3]2 and orange-brown [NbIV2(µ-S2)2(S2CNEt2)4]3 were also formed. At higher temperatures the same products were formed but a higher proportion of 1 was observed. Crystals of 2·0.5CH2Cl2 were monoclinic, space group C2/c with a= 16.360(2), b= 10.959(1), c = 30.637(3)Å, β= 92.34(1)° and Z= 8. The structure was refined to final R= 0.034 for 2310 reflections with I 2.5σ(I). The eight-co-ordinate complex exhibits an mmmm dodecahedral structure analogous to that of its tantalum counterpart.