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100 ml toluene were added and the two-phases mixed vigorously for a short time. The
organic layer was then separated and filtered through a folded filter before removing
the solvent under reduced pressure. The resulting yellow highly viscous product was
dried under vacuum at 60 °C for around 24 h and with several times lyophilizing.
Yield:
2.49 g (0.59 mmol, 60% based on K
8
[
J
-SiW
10
O
36
])
EA
in wt. - % (calculated values in brackets): C 35.02 (31.66), H 6.54 (5.79), N 1.41 (1.32)
IR
(characteristic bands in cm
-1
): 3485 (m), 2955/2928/2857 (s), 1481 (m), 1458 (m),
1379 (m), 1001 (m), 961 (m), 907 (s), 806 (s), 725 (m), 708 (m), 662 (w), 548 (w), 529 (w)
UV-Vis spectra:
Figure 61
UV-Vis spectrum of (Q
7
)
4
[
D
-SiW
10
O
36
Cu
2
(H
2
O)
2
]
in CH
2
Cl
2
. Left: c = 19.0
P
M, the extinction
coefficient is
H
226
= 32674 M
-1
cm. Right: c = 19.0 mM, the extinction coefficient is
H
724
= 27 M
-1
cm
-1
.
5.3.3 The Dawson-type Clusters
5.3.3.1
DE
-
K
6
[P
2
W
18
O
62
]
ڄ
19H
2
O (+ K
14
NaP
5
W
30
O
110
)
In the course of this synthesis the use of metal spatulas was avoided as these may
reduce the clusters!
250 g (0.76 mol) of Na
2
W0
4
ڄ
2H
2
0 were dissolved in 450 ml of water and 210 ml
(3.09 mol) of orthophosphoric acid (85%) added slowly. The solution was heated at
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