Chapter 4 - Jacobs University

Chapter 9
Unpublished Results
9.2.2 Synthesis of Na 23 [{Y (B-a -
SbW 9 O 33 )} 3 (CH 3 COO) 3 (WO 4 )]·51H 2 O (16a)
A 1.88 g (0.75 mmol) sample of Na 9 [a-SbW 9 O 33 ]∙27H 2 O and 0.228 g (0.75 mmol) YCl 3 ∙6H 2 O
was dissolved in 20 mL of 1 M LiCH 3 COO (5.3 pH) and then 0.0825 g (0.25 mmol)
Na 2 WO 4·2H 2 O was added to the resulting reaction mixture. This solution was heated to 80 °C
for 60 minutes. After heating the solution was then filtered hot. The resulting solution was
layered with 1 mL of 1 M NH 4 Cl. The filtrate was allowed to evaporate in an open beaker at
room temperature. After one week a yellow 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: 1.563g (23%). IR : 1628(s), 1543(s),
1460(w), 933(m), 897(sh), 838(m), 784(m), 681(sh) cm -1 .
65
60
55
50
45
40
%Transmittance
35
30
25
20
15
10
5
0
-5
-10
1800
1600
1400
1200
Wavenumbers (cm-1)
1000
800
600
Figure 9.27 FT-IR spectrum of 16a.
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