Chapter 4 - Jacobs University

Chapter 4
16-Iron Metal Center Nanocluster
days, washed with a small amount of cold water and dried in air. Yield: 0.09 g, 13% (based on
P 8 W 48 ); elemental analysis calcd (%) for 2b: Na, 1.30; K, 2.71. Found: Na, 1.3; K 2.8. The
identity of 2b was established by elemental analysis (in part done by Mikroanalytisches Labor
Egmont Pascher, see above), IR and complete single crystal X-ray structure analysis.
Method 5 (Bielefeld). K 28 Li 5 [H 7 P 8 W 48 O 184 ]∙92H 2 O (0.35 g, 0.024 mmol)was dissolved in 1M
NaCH 3 COO/CH 3 COOH buffer (20ml, pH 4.2). After FeCl 2 ∙4H 2 O (0.1g, 0.5 mmol) has been
added, the resulting solution was heated to 65°C for 12h and filtered after cooling it to room
temperature. Slow evaporation in an open Erlenmeyer at room temperature resulted in the
precipitation of dark yellowish crystals that were filtered off after 7 days, washed with a small
amount of cold water and dried in air. Yield: 0.03 g, 8%; elemental analysis calcd (%) for 2b:
Na, 1.30; K, 2.71. Found: Na, 1.3; K 2.8. The identity of 2b was established by elemental
analysis, XRD and IR.
84
82
80
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74
72
70
%Transmittance
68
66
64
62
60
58
56
54
52
50
48
46
1300
1200
1100
1000
900
800
Wavenumbers (cm-1)
700
600
500
Figure 4.1 FTIR spectra of compounds 2a.
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