Synthesis and Structural Characterization of ... - Jacobs University

Chapter 4
Unpublished Results
iron(III) containing phosphotungstates [Fe 16 O 2 (OH) 23 (H 2 O) 9 P 8 W 49 O 189 Ln 4 (H 2 O) 19 ] 11−
reported herein.
4.2. Synthesis
The precursor P 8 W 48 used for the synthesis of the reported species was synthesized according
to the published procedure by Contant and Tézé. 5
K 8.5 Na 0.5 Li 0.5 Eu 0.5 [P 8 W 49 O 189 Fe 16 O 2 (OH) 23 (H 2 O) 9 Eu 4 (H 2 O) 20 ]·70H 2 O (KLiNa-24)
0.17 g (0.625 mmol) of FeCl 3·6H 2 O and 0.11 g of EuCl 3·6H 2 O (0.300 mmol) were dissolved
in 20 mL of LiCH 3 COO/CH 3 COOH buffer (1M, pH 4.0). Then 0.37 g of
K 28 Li 5 [H 7 P 8 W 48 O 184 ]·92H2O (0.025 mmol) was added, followed by 25 drops of 30% H 2 O 2 .
The mixture was heated to 80 ºC for 1 hour with vigorous stirring and filtered while hot. After
cooling to room temperature, 0.5 mL NaCl (aq) was added to the filtrate which was kept in an
open vial for crystallization. Reddish brown crystals were obtained after a month, which were
filtered off and air-dried (yield 0.04 g, 10.0 %). IR data for KLiNa-24: (1069 (s), 1020 (w),
948(s), 914 (w), 839 (sh), 802 (w), 737 (m), 622 (w), 558 (w), 520 (w), 412 (w)) cm -1 . Anal.
Calcd (%) KLiNa-24: P, 1.5; W, 54.8; Fe, 5.4; Eu, 4.2; Li, 0.1; K, 2.2. Found (%):P, 1.5; W,
54.7; Fe, 5.3; Eu, 4.3; Li, 0.2; K, 2.2, Na,