Chapter 4 - Jacobs University

Chapter 9
Unpublished Results
9.2.4 Synthesis of K 12 [{Y(CH 3 COO)GeW 11 O 39 } 2 ]·37H 2 O (18a)
A 1.313 g (0.4 mmol) sample of K 8 [a-GeW 11 O 39 ]∙12H 2 O was dissolved in 25 mL of 1M
KCH 3 COO (4.8 pH) and then reacted with 0.1344 g (0.4 mmol) YCl 3 ∙6H 2 O. This solution was
heated to 80 °C for 30 minutes. After the heating was over, the solution was allowed to cool to
room temperature, and then filtered. 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 one day 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: 1.006 g. (37%). IR : 1622(s),
1533(s), 1457(s), 952(s), 881(m), 814(m), 683(m), 526(m), 469(w), 449(w) cm -1 .
75
70
65
60
55
50
%Transmittance
45
40
35
30
25
20
15
10
5
-0
1800
1600
1400
1200
Wavenumbers (cm-1)
1000
800
600
Figure 9.40 FTIR spectrum of 18a.
192