The TTF-CA crystals with and without 13C-labeling were prepared by a co-sublimation method; a vacuum-sealed glass tube containing the powdered components in the ends separately was heated with a three-zone temperature-controlled furnace. For 13C-NMR measurements, we synthesized 13C-enriched TTF molecules, in which the central double-bonded carbon atoms were substituted by 13C isotopes (Fig. 1A), according to methods described in the literature (43, 44) with slight modifications from 13CS2 (ISOTEC, 13C = 99.9 atomic %) as a starting compound. The detail of the scheme is described in fig. S2.

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