P Chemical Shift Measurements of Tungstophosphates

A 250-mL beaker fitted with a magnetic stirrer is charged with 8.2 g( 100 mmol) of sodium acetate and 100 g of water, and the mixture is stirred until the solid is dissolved. Approximately 6mL of acetic acid is added until pH 4.8 

HEXACESIUM PENTATUNGSTODIPHOSPHATE, Cs6[P2Ws023] AND HEPTACESIUM DECATUNGSTOPHOSPHATE, Cs7[PW,o036] 

In a 600-mL beaker, 60 g (0.24 mol) of tungstic acid (H2 WO4) is slurried with 400 g of water. Approximately llOmL of 50% aqueous cesium hydroxide (CsOH) is added dropwise with vigorous stirring. The turbid solution is passed through a cake of 10 g Celite Analytical Filter aid in a medium fritted filter, to produce a clear colorless solution. Phosphoric acid (85%H3P04) is added dropwise while stirring to adjust the pH to 7.0 ( 21 mL total), and the solution is stirred for an additional 1 h. The solution is filtered to produce lOg of uncharacterized product. The nitrate is cooled 

A 250-mL round-bottomed flask fltted with a reflux condenser is charged with 150g of water and 75g of Cs6[P2W5023] H20, and the contents are heated at reflux for 24 h. The solution is filtered hot through a medium frit to yield 18g of Cs7[PW,o036]-H20. The nitrate is cooled for 48 h at 0°C it is then filtered to recover 45 g of unconverted Cs6[P2W5023], which is used again in later preparations. The IR spectrum is a clear indicator of the purity and identity of all products. 

Heteropoly and Isopolymetalates, Springer-Verlag, New York, 1983. 

In a 500-mL beaker, 10g (3 mmol) of Cs5[y-PV2W,o04o] is stirred with 300 mL of water for 60 h. The solution is eooled to 0°C and passed through a cake (lOg) of Celite Analytical Filter Aid. The solution is reduced in volume to 75 mL by rotary evaporation and then cooled for I h at 0°C to produce a precipitate. Solid Cs5[ -PV2W,o04o] (8.5 g, 70%) is collected by suction filtration. The product is dissolv in 200mL of water at 25 °C (some turbidity remains as a result of undissolved impurity). The solution is passed through a filter cake of Celite Analytical Filter Aid and the filtrate is stripped to dryness to yield 7g (60% overall) of pure compound. 

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