The redox behaviour of films deposited on roughened gold electrodes in strongly alkaline solutions containing Ni-tetraazamacrocyclic complexes was monitored by potential-dependent surface-enhanced Raman scattering spectra in conjunction with cyclic voltammetry. Spectra were recorded on modified electrodes and during the procedure of electrode modification. It has been found that the complexes studied do not decompose in the procedure of modification and that they are attached to the electrode surface and interconnected via the ore-bridges.