Chapter 4 - Jacobs University

Chapter 9
Unpublished Results
9.2 Yttrium-containing Polyoxometalates
9.2.1 Synthesis of Na 23 [Cs{Y(B-a-AsW 9 O 33 )} 4 ]·58H 2 O (15a)
A 0.493 g (0.2 mmol) sample of Na 9 [B-a-AsW 9 O 33 ]∙27H 2 O was dissolved in 20 mL of 1M NaCl
and then 0.0606 g (0.2 mmol) YCl 3 ∙6H 2 O was added to the solution. The pH of reaction mixture
was 6.7. This solution was heated to 50 °C for 30 minutes and filtered it 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 week product consisting of colorless crystalline needles
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: 0.375 g
(18%). IR : 973(sh), 944 (s), 889 (vs), 789 (m), 735 (sh), 710 (s), 534 (m), 476 (w), 445 (w) cm -1 .
84
82
80
78
76
%Transmittance
74
72
70
68
66
64
62
60
1100
1000
900
800
Wavenumbers (cm-1)
700
600
500
Fig.9.24 FTIR spectrum of 15a.
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