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). The CV experiments are performed using an electrochemical setup consisting of an Autolab potentiostat (mAutolab, TYPE III) or an IVIUM CompactStat potentiostat and a three-electrode cell in which a platinum or glassy carbon disk electrode (2 mm diameter, Metrohm) serves as a working electrode. Platinum wires are used as a counter electrode and a pseudo-reference electrode, and the ferrocenium/ferrocene couple is typically employed as an internal reference standard. Scan rates commonly vary between 25 - 1600 mV/s.