A dichloromethane dispersion of Co-1-6, Homo-1, or Homo-3 was dropcast on a transparent SnO2 electrode so that the polymer was deposited in the range of a 5-mmØ circle. The coordination polymer deposited on the SnO2 electrode was always subjected to UV/vis spectroscopy before the photovoltaic conversion experiment. The baseline of the UV/vis spectrum was corrected to exclude the effect of light scattering caused by the coordination polymer film. The modified SnO2 electrode was used as a working electrode (photoanode). A homemade Ag+/Ag reference electrode (0.01 M AgClO4 in 0.1 M Bu4NClO4/acetonitrile for Co-1-6 and Homo-3) and a Pt wire counter electrode were implemented to establish a three-electrode system. The three electrodes were assembled into a photoelectrochemical cell in the same way as in the previous work (38). The cell was filled with an acetonitrile solution of Bu4NClO4 (0.1 M, as a supporting electrolyte) containing triethanolamine (TEOA; 0.05 M, as a sacrificial donor reagent). As for Homo-1, aqueous sodium sulfate (0.1 M) containing 0.03 M TEOA as an electrolyte solution and an Ag/AgCl reference electrode were used because of good dispersibility of Homo-1 in acetonitrile. The photoelectrochemical cell was sealed and deoxygenized by Ar bubbling for 5 min before the measurement. Monochromatic light for the acquisition of the action spectrum shown in fig. S7 (C to E) (450 to 600 nm in every 10 nm) was extracted from Xe lamp (MAX-302, Asahi Spectra Co. Ltd.), the photon flux of which was monochromated by a monochromator (CT-10, JASCO Corporation). For the photocurrent response shown in fig. S7B, monochromic light was provided by a Xe lamp equipped with a band-pass filter (500 nm). The active area of the electrode was fixed at 0.264 cm2, which was determined by a fluorocarbon rubber O-ring. The electrode potential was controlled using an electrochemical analyzer (ALS-750A, BAS Inc.). The potential of the photoanode was fixed at near the open circuit potential such that a negligible dark current was observed. The photocurrent was also collected through the electrochemical analyzer.

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