To a solution of (NH4)2[MoS4] (1.00 g, 3.84 mmol) in H2O (35 mL) were alternatingly added (1 mL each addition) aqueous HCl (6 M, 15 mL) and aqueous NaBH4 (2 M, 15 mL). The brown reaction mixture was heated to 90 °C while air was passed through a glass syringe. After 22 h, a colour change to dark green was observed, and the mixture was cooled with an ice bath. Filtration and washing of the filter cake with aqueous HCl (1 M, 10 mL) afforded a green filtrate condensed in vacuo to roughly 5 mL. The crude product was purified over a Sephadex G-10 (10 g, bloomed