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electrochemistry
To
elucidate the electronic structure as well as
to fully characterize the novel compounds we routinely
measure the redox properties of the molecules
in solution. In a simple voltammetric experiment
we gain important information about accessible
oxidation states of the complexes. Cyclic voltammetry
(CV) is usually performed under a dinitrogen atmosphere
(binding posts at the glove-box allow electrochemical
experiments in the glove box) in dry solvents
like acetonitrile or THF containing a pre-dried
and recrystallized electrolyte such as tetra-n-butyl
ammoniumperchlorate
(TBAClO4) or tetra-n-butylammoniumhexafluorophosphate
(TBAPF6). A one-cell compartment is used for the
CV measurements. This compartment is set up with
a gold, platinum, or glassy carbon disk electrode
(1.6 mm diameter, Bioanalytical Systems(BAS)),
which are usually employed as working electrodes.
A platinum or silver wire serve as counter
electrodes. The electrochemical response is collected
with the assistance of a CV-50W Voltammetric Analyzer
(BAS). The ferrocenium/ferrocene couple is used
as the internal standard (0V). Scan rates commonly
vary between 25 - 1600 mVs-1
.
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