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This study aimed to demonstrate the behavior of different complexes using IR spectroelectrochemistry (SEC), a technique that combines IR spectroscopy with electrochemistry. Four different Mn and Re catalysts for electrochemical CO₂ reduction were studied in dry acetonitrile. In the case of Mn(apbpy)(CO)₃Br (apbpy = 4(4-aminophenyl)-2,2′-bipyridine), SEC suggested that a very slow catalytic reduction of CO₂ also occurs in acetonitrile in the absence of proton donors, but at rather negative potentials. In contrast, the corresponding Re(apbpy)(CO)₃Br clearly demonstrated slow catalytic conversion at the first reduction potential. Switching to saturated CO₂ solutions in a mixture of acetonitrile and 5% water as a proton donor, the SEC of Mn(apbpy)(CO)₃Br displayed a faster catalytic behavior.