Octahedral Hexamolybdenum Halide Clusters

Submitted by CHANG-TONG YANG, DANIEL N. T. HAY, and LOUIS MESSERLE  

Checked by DAVID J. OSBORN IH, JEFFREY N. TEMPLETON, and LISA F. SZCZEPURA  

We report here an extension of this reduction methodology to the convenient preparation of chloromolybdic acid and Mo6Clx2. 

A tube furnace with a positionable thermocouple is used in conjunction with a temperature controller in order to maintain and ramp temperatures. Syntheses are performed in dual-chamber, 25 mm OD borosUicate glass ampules with 30-60 mL total chamber volume, a 14/20 or 19 2 ground glass joint at one end, and constrictions between the end reaction chamber and middle receiver chamber (for volatile byproducts) and between the middle receiver chamber and ground joint (Fig. 1). 

The checker used a 2.5 cm OD double-chamber ampule with a 15 cm length reaction chamber, a 10 cm receiver chamber, and a 0.95 cm OD end tube to which a greaseless vacuum valve was attached via a Cajon fitting. The ampule was flame sealed under vacuum between the receiver chamber and the Cajon fitting. 

---