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[16] Synthesis of [Co(L)2]2Na2[β-Mo8O26]·9H2O (1) A 25 mL
solution (Vmethanol/Vwater = 3/4) containing Co(ClO4)2·6H2O
(0.09 g, 0.25 mmol) and 2-acetylpyrazine N4-methyl
thiosemicarbazone (0.10 g, 0.5 mmol) was stirred at 60 °C
for 30 min. After cooling to room temperature, it was added
to a 10 mL aqueous solution of Na2MoO4·2H2O (0.24 g, 1.0
mmol), the pH value was maintained around 3.5 with 1.0 M
HCl under continuous stirring. Then the mixture was stirred
for 30 min at 60 °C and filtered. Black crystals of 1 were
isolated after five days. Yield: ca. 11.6% (based on Co).
Elemental analysis (%) for C32H58Co2Mo8N20Na2O35S4:
calcd C, 16.41; H, 2.50, N, 11.96, Co, 5.03, Mo, 32.76;
found C, 16.48, H, 2.63, N, 11.92, Co, 4.99, Mo, 32.67.
Synthesis of [Fe(L)2]2Na2[β-Mo8O26]·9H2O (2)
The preparation of 2 was similar to that of 1 except that
FeCl3·6H2O (0.07 g, 0.25 mmol) was used instead of
Co(ClO4)2·6H2O. Black crystals of 2 were collected. Yield:
ca. 12.29% (based on Fe). Elemental analysis (%) for
C32H58Fe2Mo8N20Na2O35S4: calcd C, 16.45, H, 2.50, N,
11.99, Fe, 4.78, Mo, 32.85; found C, 16.48, H, 2.59, N,
12.07, Fe, 4.71, Mo, 32.17.
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Polyoxometalate-based
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