CHE 450G: Practical Inorganic Chemistry

U of KY Dept of Chemistry

Metal-Metal Quadruple Bonds

Addenda to Girolami et. al. Experiment #11

Introduction and Background

This is the first year we are attempting this particular experiment. Therefore, additional tips and suggestions are likely to appear each week during the core experiments. Be sure to watch for updates!

Background Readings

The "Other References" listed on page 116 of your textbook are good items to consult. I have a copy of Cotton's Multiple Bonds Between Metal Atoms and will arrange to put this text on reserve as well.

Notes

1. You should complete both Part A as well as the first section of Part B (K₄Mo₂Cl₈^.2H₂O) during the assigned laboratory periods. You are not responsible for the phosphine derivative.

2. Use a magnetic stirbar and stir plate instead of boiling stones during the synthesis.

3. You may use a Schlenk flask instead of a two-necked flask as your reaction vessel in Part A.

4. Characterize your compounds by IR, UV-VIS and melting point. Be certain to explain, interpret and compare all of your data (including to previously reported values in the primary literature).
   You should be able to get the UV-VIS spectrum of at least one of these compounds in 95% ethanol. Make up your solution volumetrically in order to determine the epsilon value. Decomposition in solution can be rapid, so make up your sample at the instrument and work quickly!

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