A novel Wells–Dawson polyoxometalate-based metal–organic framework constructed from the uncommon in-situ transformed bi(triazole) ligand and azo anion

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Synthesis of 1: a mixture of AgNO3(0.15g, 0.9mmol), L′ (0.03g, 0.1mmol) α-K6P2W18O62·15H2O (0.3g, 0.1mmol), NH4VO3 (0.036g, 0.3mmol) and H2O (10mL) was stirred for 30min at room temperature. The pH value was then adjusted to about 1.0 using 1.0M HNO3. The suspension was transferred to a Teflon lined autoclave (25mL) and kept at 170°C for 5days, then the autoclave was slowly cooled to room temperature. Yellow crystals of compound 1 were filtered off, washed with distilled water, and dried in a desiccator at room temperature to give a yield of 15% based on Ag. IR (KBr pellet, cm−1): 3578 (s), 1637 (s), 1523(w), 1296 (w), 1096 (s), 914 (s), 909 (s), 790 (s), 530 (w).

Crystal data for compound 1: C24H12Ag13N38O62P2W18, FW=6598.09, Monoclinic, space group P 2/n, a=12.880(5) b=12.110(5) c=28.587(5), α=90.000(5)°, β=94.818 (5)°, γ=90.000(5)°, V=4443(3) Å, Z=2, Dcalc=4.932mg/m3, λ=0.71073Å, T=298(2) K, R1 (wR2)=0.0803 (0.2220), Bruker Smart Apex-II CCD area detector, Mo Kα radiation. The structure was solved by direct methods and refined on F2 by full-matrix least squares methods using SHELXTL 97. CCDC reference number 1062637.

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The compound 1 bulk-modified CPE (1–CPE) was fabricated by mixing 0.10g graphite powder and 0.030g compound 1 in an agate mortar for approximately 30min to achieve a uniform mixture; then 0.16mL paraffin oil was added and stirred with a glass rod. The homogenized mixture was packed into a 3mm inner diameter glass tube and the tube surface was wiped with weighing paper. The electrical contact was established with the copper wire through the back of electrode.

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