Finally, the nanofiber structure was fully analyzed by 3D electron crystallography. Needleshaped microcrystals of 1-H were collected from the supernatant of the gel obtained from a TCE solution at room temperature. As shown in Figure , the needle-shaped microcrystals were found by TEM measurement to have widths of around 0.5 µm. Electron diffraction patterns were recorded at a specimen temperature of ~98 K (Figure and SM for detail) by the electron energyfiltered diffraction (eEFD) method . A total of 46 datasets were merged, and the highresolution limit was determined to be 0.85 Å. The initial structure was successfully solved with a space group P42 by molecular replacement, starting from the structure of 1-Cl, and direct phasing also gave the same solution. As shown in Figure , the molecular structure of 1-H was confirmed as expected.