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Cathodic IR spectroelectrochemistry showing (a) ETC-conversion of [Re(3,3′-DHBPY-H+)(CO)3Cl]− (↓) at R2* (cf. Figure 4) to [Re(3,3′-DHBPY)(CO)3Cl]•– (↑) as a net-zero-electron process and (b) subsequent reduction of [Re(3,3′-DHBPY)(CO)3Cl]•– (↓) at R2 to [Re(3,3′-DHBPY-2H+)(CO)3]3– (↑). Conditions: an OTTLE cell, THF/Bu4NPF6, T = 298 K.
