Abstract
The reaction of NiCl2 · 6H2O, Na2MoO4 ċ 2H2O, and sulfur in a mixture of diethylenetriamine and 0.2 M ammonia solution (1:4) under solvothermal conditions leads to the formation of orange-red crystals of the oxothiomolybdate Ni(dien)2[Mo2O2S6] (dien = diethylenetriamine) in nearly 100% yield. The structure consists of [Ni(dien)2]2+ cations and discrete dimeric [Mo2O2S6]2− anions. The compound crystallizes in the monoclinic space group P21/c (a = 8.726(2), b = 18.111(4), c = 14.419(3) A, β = 101.686(3)°). Upon heating the compound decomposes in a single step starting at about 250°C. The final decomposition product was identified by X-ray powder diffractometry as MoS2 and Ni3S2. Spectroscopic data as well as detailed synthetic procedures for Ni(dien)2[Mo2O2S6] are reported.
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