The compounds MS(7/2-SCNEt2)(i;2-S2CNEt2)2 ( = niobium or tantalum) have been prepared from the reaction of NaS2CNEt2 with M2Cl6(SC4H8)3. These new compounds were characterized using spectroscopic methods and X-ray crystallography. NbS(SCNEt2)(S2CNEt2)2•* 1 /4C6H6 crystallizes in the triclinic space group, PI, with cell parameters of a = 10.390 (4) k,b= 14.002 (3) A, c = 18.314 (11) A, a = 104.39 (4)°, ß = 93.13 (4)°, y = 90.11 (3)°, V = 2576 (2) A3, and Z = 4. The coordination sphere of the metal(V) atom consists of a lone sulfur atom, two chelating dithiocarbamate ligands, and one thiocarbamyl ligand bound through both the carbon and the sulfur atoms. The resulting structure is a seven-coordinate pentagonal bipyramid having the lone sulfur atom and a sulfur from one of the dithiocarbamate ligands occupying the polar positions. The formation of a sulfur ligand and thiocarbamyl ligand, SCNEt2~, corresponds to the oxidative addition of one C-S bond to the metal(III) center with concomitant cleavage of the dimer. A dimeric compound with bridging tridentate dithiocarbamate ligands is proposed as a necessary intermediate for the oxidative addition reaction to occur.
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