Chapter 4 - Jacobs University

Chapter 4
16-Iron Metal Center Nanocluster
752(s), 687(s), 647(sh) [n as (W-O-W)], 559(w), 526(w), 473(w) cm -1 . Anal. Calcd for 2a: Li,
0.18; K, 4.56; Fe, 5.78; W, 57.1; P, 1.60; Cl, 0.46. Found: Li, 0.24; K, 4.73; Fe, 5.35; W, 58.1; P,
1.60; Cl, 0.28. The degree of hydration of 2a was determined by TGA (see Figure 4.2).
Elemental analysis was performed by Mikroanalytisches Labor Egmont Pascher, An der
Pulvermühle 3, 53424 Remagen, Germany.
Method 2 (Bremen). A sample of K 28 Li 5 [H 7 P 8 W 48 O 184 ]·92H 2 O (0.185 g, 0.0125 mmol) was
dissolved in 0.5 M LiCH 3 COO/CH 3 COOH buffer (20 mL) at pH 4.0. Then Fe(ClO 4 ) 3·xH 2 O
(0.0974 g, 0.275 mmol) was added and the solution was heated to 80 °C for 1h and filtered
while hot. The following steps were identical to those of Method 1. The identity of 2a (isolated
in very low yield,