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note
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5Br (0.135 g) and DMF (6 mL) is sealed in a 15 mL Teflon-lined autoclave at 160 °C for 4 days. After cooling the autoclave to room temperature for two days, red block crystals were obtained. (Yield: 75% based on W). IR spectra: 3432(s), 1646(s), 1384(m), 1110(s), 1030(m), 970(s), 937(m), 869(m), 832(m), 781(s), 743(m), 722(m), 687(m). UV sepctra: 193 nm, 250 nm.
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67349171234
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note
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int = 0.0642) reflections were measured in the range of -17 ≤ h ≤ 15, -23 ≤ k ≤ 23, -16 ≤ l ≤ 24. The structures were solved by direct methods and refined by using full-matrix least-squares calculations with anistropic thermal parameters for all non-hydrogen atoms. The hydrogen atoms were geometrically fixed to allow riding on the parent atoms to which they are attached. All calculations were performed with using the SHELXTL-97 program.
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Yu, X.Y.8
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