Air-Tight Three-Electrode Design of Coaxial Electrochemical-EPR Cell for Redox Studies at Low Temperatures
The weak point of the original Allendoerfer electrochemical-EPR cell has been the reference electrode, placed outside the space-limited electrolysis cavity or not used at all in experiments at low temperatures. We present here an elegant solution to this problem, based on a modified air-tight design...
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| Published in: | Collection of Czechoslovak chemical communications Vol. 66; no. 1; pp. 52 - 66 |
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| Main Authors: | , , |
| Format: | Journal Article |
| Language: | English |
| Published: |
2001
|
| Online Access: | Get full text |
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| Summary: | The weak point of the original Allendoerfer electrochemical-EPR cell has been the reference electrode, placed outside the space-limited electrolysis cavity or not used at all in experiments at low temperatures. We present here an elegant solution to this problem, based on a modified air-tight design of an Allendoerfer cell equipped with a silver-wire pseudoreference electrode. The cell performance is demonstrated on one-electron electrochemical oxidation of heterocyclic 3,6-diphenyl-1,2-dithiine and one-electron reduction of 6-methyl-6-phenylfulvene and the pseudo-octahedral complex
fac
-[Re(benzyl)(CO)
3
(dmb)] (dmb = 4,4'-dimethyl-2,2'-bipyridine). In the latter case, the EPR spectrum of the radical anion [Re(benzyl)(CO)
3
(dmb)]
•-
points to predominant localization of the unpaired electron on the dmb ligand, in agreement with UV-VIS and IR spectroelectrochemical data. |
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| ISSN: | 0010-0765 1212-6950 |
| DOI: | 10.1135/cccc20010052 |