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ÐèÒª´ïµ½2*10-4 torr¡£ ÔÎÄÈçÏ£º Preparation of Mo3S7CI4. Molybdenum powder (1 .OO g, 10.4 mmol), sulfur (0.34 g, 10.4 mmol), and S2CI2 (0.94 g, 6.9 mmol) were placed in a tube. The contents was degassed by three freeze-pumpthaw cycles and then sealed under a vacuum of 2 X lo-4 Torr. The tube was placed in an oven that was slowly warmed to 425 OC (over ca. 8 h) and kept there for 48 h. The oven was then turned off, and the tube was cooled to room temperature over a period of 12 h. A homogeneous mass of red crystals was formed. The product was washed with dichloromethane and dried under vacuum. The isolated yield was 1.92 g, 85% based on Mo. |
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