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A mixture of Na9[A-α-PW9O34] ·7H2O (0.246 g, 0.094 mmol, FeSO4·7H 2O (0.139 g, 0.500 mmol, en (0.05 mL, 0.740 mmol, HAc (0.10 mL, 1.748 mmol, and H2O (5 mL, 277 mmol) was stirred for 1 h, sealed in a 20 mL Teflon-lined steel autoclave, kept at 100°C for 5 days, and then cooled to room temperature. The red crystals were harvested. Yield: ca. 38% based on Na9[A-α-PW9O34]·7H 2O. Anal. Calcd, ) for C7N7H 228O247P8Fe13W36: C, 0.70; H, 1.92; N, 0.82; P, 2.07; Fe, 6.07; W, 55.36. Found: C, 0.82; H, 2.20; N, 0.76; P, 1.99; Fe, 5.98; W, 55.52. The P:Fe:W ratio observed by energy-dispersive X-ray analysis: 1:1.70:4.80. Calcd: 1:1.63:4.50. IR (KBr pellet, 3467, 3137, 1611, 1507, 1048, 947, 871, 790, 730, 476 cm-1 Figure S8 in the Supporting Informa
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-1 (Figure S8 in the Supporting Information).
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36
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38149065655
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Intensity data of 1 were collected at 293 K on a Rigaku Saturn 70 CCD diffractometer using graphite-monochromated Mo Kα radiation (λ, 0.710 73 Å, The structure was solved by direct methods and refined by full-matrix least squares on F2 using the SHELXTL-97 program package. Routine Lorentz and polarization corrections and empirical absorption correction were applied. P4, P5, and P6 atoms were disordered over two positions; Fe8 and Fe9 atoms were also disordered with an occupancy of 0.25 for each. Crystal data for 1: C7N7H 228O247P8Fe13W36, Mr, 11955.80, monoclinic, space group C2/m, a, 36.666(7) Å, b, 25.887(5) Å, c, 21.682(4) Å, β, 94.891(3)°, V, 20505(6) Å3, Z, 4, S, 1.088, R1, 0.0526, wR2, 0.1327
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3, Z = 4, S = 1.088, R1 = 0.0526, wR2 = 0.1327.
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