31P{1H} nuclear
magnetic resonance spectroscopy
is a particularly useful tool for studying the reactions of P-donor
ligands such as phosphines and phosphites with transition metals and
other Lewis bases because the reactions take place on the nonbonding
pair of electrons on the phosphorus. In addition, 31P has
a 100% natural abundance and a high gyromagnetic ratio resulting in
a high sensitivity that allows the spectra to be recorded using small
amounts of sample. An activity that combines air-sensitive synthesis
of transition metal complexes of P-donor ligands and the characterization
of these complexes with 31P{1H} NMR spectroscopy
has been developed for an upper-division, laboratory-based inorganic
course. This laboratory familiarizes students with this useful nucleus
for NMR spectroscopy and allows them to study the factors that affect
the 31P{1H} NMR chemical shifts of phosphorus-donor
ligands and their transition metal complexes. Details of the activity,
including procedure and pretest, are provided. Alternative methods
and presentations are also proposed.