rotation electron diffraction (cRED) samples were dispersed in acetone,
and a droplet of the suspension was transferred onto a carbon-coated
copper grid. Observation was performed on a JEOL JEM2100 microscope
operated at 200 kV (Cs = 1.0 mm, point resolution = 0.23 nm). Images
were recorded with a Gatan Orius 833 CCD camera (resolution 2048 ×
2048 pixels, pixel size 7.4 μm) under low dose conditions. Electron
diffraction patterns were recorded with a Timepix pixel detector QTPX-262k
(512 × 512 pixels, pixel size 55 μm, Amsterdam Sci. Ins.).
The data were collected using the software Instamatic.37 (link) A single-tilt tomography holder was used for
the data collection, which could tilt from −70 to +70°
in the microscope. The aperture used for cRED data collection was
about 1.0 μm in diameter. The speed of the goniometer tilt was
0.45° s–1, and the exposure time was 0.5 s
per frame. Three data sets were collected within 3.4, 3.5, and 3.7
min to minimize the beam damage and to maximize the data quality.
The covered tilt angles are 91.71, 94.56, and 99.95°, respectively.
In order to increase the completeness, these data sets were merged
via using XDS package.64 (link)