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34
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4243170448
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note
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3. The mixture was allowed to warm to room temperature over 1.5 h and further stirred at room temperature for 17 h. A grey solid was filtered off and washed copiously with pentane. The filtrate and the washings were combined and concentrated to ca. 10 mL, and the solution was kept in a freezer for 1 day. After filtration of the dark green crystals at -78 °C and washing with cold pentane, the solid was recrystallized from pentane to give 1 in 22-38% yield.
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35
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85085781299
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note
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3, Z = 16, space group Pbcn, R = 5.06%, GOF = 1.16.
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39
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85085781415
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note
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ii parameters were taken from the following: Moore, C. Circular 467 U.S. Department of Commerce, National Bureau of Standards, Vol. 1, 1949.
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40
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85085780866
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note
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3 groups of 1 were replaced by H atoms with a Si-H distance of 1.48 Å.
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