Bis hydroxonium Tetradecachlorohexatungstate Heptahydrate Chlorotungstic Acid

6WC16 + 8Bi - W6CI12 + SBiCls WfiClia + 2HCl(aq) (H30)2[W6(tt3-Cl)gCl6] THjO 

WCls (15.00 g, 37.8 mmol) and Bi (10.54 g, 50.4 mmol) are mixed in the glove box and sealed in an ampule under vacuum. The ampule is positioned at the tube furnace center and the temperature slowly raised to 230° C over 2h, and then to 355° C over 2h. The ampule is then positioned with the receiver chamber in a cooler area of the furnace and heated at the reaction chamber end at 350-355° C for 24 h. After being cooled to room temperature, the ampule is opened in the glove box, taking care not to mix any nonvolatile material and BiCls from their respective chambers. Alternatively, before opening the ampule, the two chambers can be separated with a torch in order to separate/store the sublimed BiCls. The chocolate brown nonvolatile material weighs 18.28 g, consistent with appreciable bismuth content because the theoretical yield of WeCl is 9.64 g. 

A portion of the chocolate brown product (3.00 g) is treated with concentrated aqueous HCl (5 mL) while agitating for 10-15 min at room temperature. This step results in the formation of a fine, yeUow-brown precipitate. The precipitate is separated by decanting off the liquid, and then the precipitate is washed with concentrated HCl (5mL) and dissolved in boiling concentrated HCl (20 mL). When the solution cools to room temperature, greenish yellow needles form. The needles are collected by filtration through a coarse porosity fritted glass funnel. The 

for H20O9CI14W6 (HsOaiWeCpa-COgClg] THaO W, 62.55. Found W, 62.41. 

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