Chapter 4 - Jacobs University

Chapter 9
Unpublished Results
Chapter 9
Unpublished Results
9.1 Interaction of metal ions with [H 7 P 8 W 48 O 184 ] 33-
9.1.1 Synthesis of K 12 Li 13 [Cu 20 Br(OH) 24 (H 2 O) 12 (P 8 W 48 O 184 )]·81H 2 O
(6a)
A sample of CuBr 2·2H 2 O (0.171g, 0.66 mmol) was dissolved in a 1M LiCH 3 COO buffer solution
(20mL) at pH 6.0, then K 28 Li 5 [H 7 P 8 W 48 O 184 ]·92H 2 O (0.37g, 0.025mmol) was added. This
solution was heated up at 80 °C for 1h and filtered in hot. The filtrate was allowed to evaporate
in an open beaker at room temperature. After one day a blue crystalline product started to
appear. Evaporation was allowed to continue until the solution level had approached the solid
product, which was then collected by filtration and air-dried. Yield: 0.18g (35%) IR: 1120(s),
1079(s), 1017(m), 950(sh), 935, 902, 835, 752, 680, 525, 471cm -1 .
65
60
55
50
45
%Transmittance
40
35
30
25
20
15
10
5
1200
1100
1000
900
800
Wavenumbers (cm-1)
700
600
500
Figure 9.1 FT-IR spectrum of 6a.
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