Chapter 4 - Jacobs University

Chapter 9
Unpublished Results
9.1.3 Synthesis of K 12 Li 13 [Cu 20 N 3 (OH) 24 (H 2 O) 12 (P 8 W 48 O 184 )]·28H 2 O
(8a)
A sample of CuSO 4·5H 2 O (0.082 g, 0.33 mmol) was dissolved in a 1M LiCH 3 COO buffer
solution (20 mL) at pH 6.0, then K 28 Li 5 [H 7 P 8 W 48 O 184 ]·92H 2 O (0.185 g, 0.0125 mmol) was added
and then NaN 3 (0.076 g, 1.16 mmol) was also added to this reaction mixture. The solution was
heated up at 80 °C for 1h and the solution was filtered hot. The filtrate was allowed to evaporate
in an open vial at room temperature. After 5-6 days later a blue crystalline product started to
appear. Evaporation was allowed to continue until the solution level reached the solid product,
which was then collected by filtration and air-dried. IR: 1137(sh),1120(s), 1080(s), 1016(m),
951(sh), 933(s), 908(m), 830(sh), 754(s), 681(s), 523(w), 472(w) cm -1 .
75
70
65
60
%Transmittance
55
50
45
40
35
1200
1100
1000
900
800
Wavenumbers (cm-1)
700
600
500
Figure 9.7 FT-IR spectrum of 8a.
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