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0011392867
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note
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2S vaporized. The solid that formed was filtered, and the solvent was removed under vacuum. Benzene (10 mL) was added to the crude product. After a second filtration and slow crystallization at room temperature 1 (0.14 g, 0.16 mmol, 27%) was obtained as colorless crystals, suitable for an X-ray crystal structural analysis. For the other analytical investigation the crystals were ground and stored under vacuum for 5 h to remove the benzene.
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19
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0011483134
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note
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12 (878.20): C, 38.3; H, 8.7. Found: C, 37.5; H, 8.8.
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20
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0011394939
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note
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2 on all data by full-matrix least squares with SHELXL-97. All non-hydrogen atoms were refined anisotropically. All hydrogen atoms were included in the model at geometrically calculated positions and refined using a riding model. Other details of the data collection, structure solution, and refinement are listed in Table 1.
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21
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Sheldrick, G.M.1
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