Chemistry Reference
In-Depth Information
Figure 59
UV-Vis spectrum of (Q
8
)
5
[
D
-SiW
11
O
39
Fe(H
2
O)] in CH
2
Cl
2
(c = 9.3
P
M). The extinction coefficient is
H
263
= 58976 M
-1
cm
-1
.
5.3.1.6 (Q
7
)
4/5
[
D
-PW
11
O
39
M(H
2
O)] M = Cu
II
/Fe
III
For the synthesis of (Q
7
)
5
[
D
-PW
11
O
39
Cu(H
2
O)] an excess of CuCl
2
ڄ
2H
2
O (1.00g,
5.87 mmol) was dissolved in 40 ml of water, together with 5.00 g (15.16 mmol)
Na
2
WO
4
ڄ
2H
2
O. After addition of 40 ml of 1M H
3
PO
4
a temporary blue precipitate
formed which completely dissolved again after stirring the reaction mixture for 10
minutes. Afterwards 4.3 eq. of Q
7
-Br (2.94 g, 6.00 mmol) in 60 ml of toluene were
added. In the biphasic system the organic layer turned orchid at first and lime green
after shaking in the separation funnel. The organic layer was separated solvent stripped
once with 50 ml toluene and the solvent removed partially. The product then formed a
separate dark lime green colored phase as the bottom layer with the aqueous layer as
light lime green colored top layer. Under vacuum the biphasic system was completely
removed of solvent and dried there for 3 d with several times lyophilizing.
Yield:
2.627 g (0.55 mmol, 39.6% based on Na
2
WO
4
ڄ
2H
2
O)
EA
in wt. - % (calculated values in brackets): C 33.09 (34.94), H 5.98 (6.32), N 1.23 (1.46)
IR
(characteristic bands in cm
-1
): 3449 (m), 2955/2928/2857 (s), 1481 (m), 1460 (m),
1096 (m), 1070 (w), 1054 (w), 1026 (m), 962 (s), 878 (m), 820 (m), 798 (w), 750 (w), 662
(w), 606 (w), 548 (w), 529 (w)
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