Chemistry Reference
In-Depth Information
entry
No.
formula
T range of
'
m (II)
(°C)
m
0
of
sample
(mg)
'
m (I)
(%)
'
m (II)
(%)
N (cations)
calculated
(Q
5
)
6
[D-SiW
11
O
39
Cu(H
2
O)]
1
200-420
53.539
3.7
39.1
6.16
(Q
5
)
5
[D-SiW
11
O
39
Fe(H
2
O)]
2
210-420
25.542
3.9
38.1
5.61
(Q
6
)
6
[D-SiW
11
O
39
Cu(H
2
O)]
3
200-415
61.617
2.9
44.1
6.23
(Q
6
)
5
[D-SiW
11
O
39
Fe(H
2
O)]
4
205-415
33.474
1.3
37.3
5.08
(Q
7
)
6
[D-SiW
11
O
39
Cu(H
2
O)]
5
210-430
74.235
4.5
46.5
6.19
(Q
7
)
6
[D-SiW
11
O
39
Co(H
2
O)]
6
195-405
40.279
2.6
43.5
6.18
(Q
7
)
6
[D-SiW
11
O
39
Ni(H
2
O)]
7
200-405
72.857
11.0
41.4
5.91
(Q
7
)
6
[D-SiW
11
O
39
Mn(H
2
O)]
8
200-410
59.270
6.8
45.0
6.13
(Q
7
)
5
[D-SiW
11
O
39
Fe(H
2
O)]
9
205-410
75.805
6.4
43.1
5.38
(Q
7
)
5
[D-SiW
11
O
39
Cr(H
2
O)]
10
200-405
19.517
8.6
43.5
5.56
(Q
8
)
6
[D-SiW
11
O
39
Cu(H
2
O)]
11
190-400
29.210
2.4
46.4
6.14
(Q
8
)
5
[D-SiW
11
O
39
Fe(H
2
O)]
12
195-400
31.631
3.7
44.3
5.01
Table 4
Thermogravimetric analysis for compounds 1-12, showing the mass loss steps and number of
cations observed.
From the calculated amount of cations their stoichiometric number and therefore the
successful cluster synthesis and its practically quantitative phase transfer is confirmed.
All calculated values N show slightly higher values than their respective stoichiometric
number because small amounts of residual solvent may still contribute to the weight
loss at higher temperatures (e.g. cluster bound water; see also the discussion of IR-data
in chapter 3.1.3.1). Additionally, small amounts of the thermally stable cluster can be
carried away under the influence of heat and the gas stream, also adding weight loss to
'
m(II) additionally to the loss of Q
y
, why slightly higher values are not only reasonable
but to be expected for the calculated number of counterions N.
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