Chapter 4 - Jacobs University

Chapter 9 Unpublished Results
9.2.5 Synthesis of K 13 [Y(SiW
11 O 39 ) 2 ]·25H 2 O (19a)
A 0.644 g (0.2 mmol) sample of K 8 [SiW 11 O 39 ]∙13H 2 O was dissolved in 20 mL of 1M KCH 3 COO
(4.8 pH) and then reacted with 0.0667 g (0.2 mmol) YCl 3 ∙6H 2 O. This solution was heated to 80
°C for 60 minutes. After that, 2 mL of 30% hydrogen peroxide (1 mmol) was added to the hot
solution. After heating, the solution was then filtered in hot. The resulting solution was layered
with 0.5 ml of 1 M CsCl. The filtrate was allowed to evaporate in an open beaker at room
temperature. After about three days a white crystalline product started to appear. After that, the
evaporation was allowed to continue until the solution level approached the solid product which
was then collected by filtration and air dried. Yield: 0.489g (39%). IR (cm -1 ): 1035(w), 1005(sh),
956(s), 908(vs),7 60(s), 725, 625 (sh), 540, 520, 472(sh), 430(sh).
Figure 9.47 FTIR spectrum of 19a.
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