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note
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2O (12 mL) was stirred for 0.5 h in air, then transferred and sealed in a 25 mL stainless-steel container with a Teflon liner, which was heated at 160 °C for 72 h and then slowly cooled to room temperature. The pale yellowish crystal was obtained by filtration, washed with ethanol and water, for 1 yield 56% and for 2 62%. Elem. anal. for 1, calcd. C 46.31, H 3.24, N 9.00; found C 46.21, H 3.28, N 9.10; For 2, calcd. C 46.17, H 3.23, N 8.97; found C 46.10, H 3.19, N 9.05.
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22
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33846927731
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note
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2 using the SHELXTL-97 program. All non-hydrogen atoms were refined anisotropically. The hydrogen atoms were generated geometrically and treated by a mixture of independent and constrained refinement.
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