Chromatographic grade acetonitrile

All the reactions were performed in argon unless otherwise mentioned. All the solvents were of analytical grade and distilled before use. IrCl₃•3H₂O and Coumarin 6 was purchased from Sigma-Aldrich. 2-Phenylpyridine, NH₄PF₆, and N-iodosuccinimide were purchased from HEOWNS. Triphenylphosphine, dichlorobis(triphenyl-phosphine)palladium(II), CuI, and 2,2'-bipyridine were purchased from Adamas-beta. Chromatographic-grade acetonitrile was purchased from Adamas Reagent. The synthetic scheme of Ir-1–Ir-4 is presented in Supplementary Fig. 1. The synthetic intermediates and target complexes were evidenced by ¹H NMR and mass spectroscopy.

All the reactions were performed in argon unless otherwise mentioned. All the solvents were of analytical grade and distilled before use. The dichloro(p-cymene)ruthenium(II) dimer and 1,10-Phenanthroline were purchased from Sigma-Aldrich. The 1-pyrenylboronic acid, NH₄PF₆ and K₂CO₃ were purchased from HEOWNS. The Tetrakis(triphenylphosphine)palladium(0) and CuI were purchased from Adamas-beta. Chromatographic-grade acetonitrile was purchased from Adamas Reagent. The synthetic scheme of Ru-1–Ru-4 is presented in Supplementary Scheme 1. The synthetic intermediates and target complexes were evidenced by ¹H NMR, ¹³C NMR and mass spectroscopy. Elemental analysis was performed as C/H/N analyses on the Vario EL Cube (Elementar, Germany).
Electrochemical measurements were carried out on a CHI 760E electrochemical workstation at room temperature. The amount of CO product was analysed by gas chromatography (Shimadzu GC-2014+AT 230C, TDX-01 column, TCD, argon carrier). UV-vis absorption spectra were recorded on a LAMBDA750 UV-vis spectrophotometer. Fluorescence spectra were taken on a Hitachi F4600 spectrofluorometer. Transient absorption spectra were measured on the LP980 laser flash photolysis instrument (Edinburgh, UK).