VERSATILE CRYOSTATED OPTICALLY TRANSPARENT THIN-LAYER ELECTROCHEMICAL(OTTLE) CELL FOR VARIABLE-TEMPERATURE UV-VIS IR SPECTROELECTROCHEMICAL STUDIES

This article describes the construction of a novel optically transpare nt thin-layer electrochemical (OTTLE) cell for IR and W-Vis spectroele ctrochemical experiments at variable temperature. The cell has a three -electrode set melt-sealed into a smooth polyethylene spacer which is sandwiched between two CaF2 windows. The width of this spacer (0.18-0. 20 mm) defines the thickness of the thin solution layer. The whole ele ctrode assembly is housed in a thermostated Cu block of the OTTLE cell which fits into a double-walled nitrogen-bath cryostat. The experimen tal setup permits relatively fast electrolysis within the tested tempe rature range of 295 to 173 IC under strictly anaerobic conditions and protection of light-sensitive compounds. Other important merits of the cell design include lack of leakage, facile cleaning, almost negligib le variation of the preset temperature, and facile manipulation in the course of the experiments. The applicability of the variable-temperat ure IR/UV-Vis OTTLE cell is demonstrated by stabilization of a few ele ctrogenerated carbonyl complexes of Mn(I) and Ru(II) with 3,5-di-tert. butyl-1,2-benzo(semi)quinone (DB(S)Q) and N,N'-diisopropyl-1,4-diaza- 1,3-butadiene (iPr-DAB) ligands, respectively, at appropriately low te mperatures.