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25
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70349418784
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note
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3 with stirring. Finally, 440 mg of dabco was added slowly to the above mixture. After stirring for 30 min, the mixture was transferred into a sealed Teflon-lined steel autoclave and heated at 160 °C for 3 days, then cooled to room temperature. Colorless plate-like crystals of compound 1 were collected and air-dried at room temperature (68% yield based on Indium). The purity of 1 was confirmed by comparison of the experimental powder X-ray diffraction pattern to the calculated spectrum based on the single-crystal structure (as shown in Fig. S1). The diffraction peaks on both spectra correspond well in position, indicating the phase purity of the as-synthesized sample.
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26
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70349418789
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note
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2 using SHELXTL 5.1 software package [27]. Firstly, the In and P atoms were located, followed by location of the framework oxygen and carbon atoms. Subsequently, non-framework carbon and nitrogen atoms were located in difference Fourier maps. The hydrogen atoms from the framework and guest molecules were initially located from difference Fourier maps; however for the final refinement they were placed geometrically. Lastly, all non-hydrogen atoms were refined anisotropically.
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27
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70349412220
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G.M. Sheldrick, SHELXTL-NT, Version 5.1, Bruker AXS Inc. Madison, WI, 1997
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G.M. Sheldrick, SHELXTL-NT, Version 5.1, Bruker AXS Inc. Madison, WI, 1997.
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