We report the synthesis of a rigid phosphine-substituted, redox-active pincer ligand and its application to electrocatalytic CO 2 reduction with first-row transition metal complexes. The tridentate ligand was prepared by Stille coupling of 2,8-dibromoquinoline and 2-(tributylstannyl)pyridine, followed by a palladium-catalyzed cross-coupling with HPPh 2 . Complexes were synthesized from a variety of metal precursors and characterized by NMR, high-resolution mass spectrometry, elemental analysis, and cyclic voltammetry. Formation of bis-chelated metal complexes, rather than mono-chelated complexes, was favored in all synthetic conditions explored. The complexes were assessed for their ability to mediate electrocatalytic CO 2 reduction, where the cobalt complex was found to have the best activity for CO 2 -to-CO conversion in the presence of water as an added proton source.