13C-NMR measurements were conducted for a 13C-labeled TTF-CA single crystal in a magnetic field H of 8 T applied parallel to the a axis (corresponding to the 1D direction). In this field configuration, all TTF molecules are equivalent against H, and thus, we observed two peaks arising from dipole interactions between the two 13C nuclei on the double-bonded sites. We used a solid-echo pulse sequence to obtain the NMR signals. The spectra shown in Fig. 3A were acquired at the time tj of 5T1 to 10T1 after the saturation of nuclear magnetization except for the measurements at 3 kbar; at such a low pressure, T1 at 13C site was too long to fulfill the ideal condition of tj > 5T1, and thus, tj was inevitably set to times comparable to T1. The spin-lattice relaxation rate 13T1−1 was determined by fitting the single exponential function to the relaxation curve. To apply hydrostatic pressure to the sample, we used clamp-type pressure cells built using nonmagnetic BeCu with Daphne 7373 as a pressure medium. The conversion coefficient from applied to internal pressures is the same as in the 1H-NMR measurements.

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