Preparation of a Molybdenum-Phosphine Complex containing a Mo-Mo Quadruple Bond

Last Update: August 18, 2006

This synthesis is from Girolami et al.¹  Take care in the synthesis of Mo₂(O₂CCH₃)₄ that you do not clog the condenser.  You should also be aware that the acetate is relatively unstable and should be converted into the chloride as soon as possible.  The chloride is also not particularly stable when left in air for long periods of time. 

The phospine that you will use will depend on which one we can obtain before the end of the semester.  Note that ¹H NMR will be very useful in characterizing the phosphine complex (you may even want to try ³¹P NMR, if time permits).

Reference

1. Girolami, G. S.; Rauchfuss, T. B. and Angelici, R. J. Synthesis and Techniques in Inorganic Chemistry: A Laboratory Manual 3^rd Ed.; University Science: Sausalito, CA, 1999, Experiment 11.

 

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