Preparation and NMR Spectroscopy of a Series of Iridium Compounds with Interesting Ligand Combinations: An Advanced Undergraduate Experiment in Organometallic Chemistry

TCE

The Chemical Educator

ISSN: 1430-4171 (electronic version)

Table of Contents

Abstract Volume 13 Issue 6 (2008) pp 353-357

Preparation and NMR Spectroscopy of a Series of Iridium Compounds with Interesting Ligand Combinations: An Advanced Undergraduate Experiment in Organometallic Chemistry

Jason Cooke*

Department of Chemistry, University of Alberta, Edmonton, AB, Canada, T6G 2G2 jason.cooke@ualberta.ca
Received June 6, 2008. Accepted November 18, 2008.

Published online: 1 December 2008

Abstract. An advanced undergraduate laboratory experiment in organometallic chemistry is described. A series of iridium compounds containing interesting ligand pairings (hydride/olefin, hydride/aqua, hydride/dihydrogen) can be readily prepared from [Ir(COD)(PPh₃)₂]BF₄, which in turn can be easily synthesized from [Ir(COD)Cl]₂. The latter starting material is obtained in good yield using microwave-assisted reflux, and strategies are presented for working as efficiently as possible with the precious iridium compounds that are prepared. The investigated compounds all provide useful models for the interpretation of NMR spectra, and research-oriented techniques are introduced such as microscale chemistry, low temperature NMR experiments, and NMR tube reactions.

Key Words: Laboratories and Demonstrations; inorganic chemistry; iridium; organometallics; catalysis; NMR spectroscopy

(*) Corresponding author. (E-mail: jason.cooke@ualberta.ca)

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