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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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ssdyok: ½ð±Ò+1 2012-12-13 18:46:59
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