Crystal structure of copper perchlorophthalocyanine analysed by 3D electron diffraction

The structure of copper perchlorophthalocyanine (CuC32N8Cl16, Pigment Green 7) was solved from three-dimensional electron diffraction data (3D ED) and placed into the series of known copper phthalocyanine crystal structures.


Contents
Continuous electron diffraction data collection 1 Technical data of all collected 3D ED datasets 2 On electron dose distribution during 3D ED data collection static patterns vs continuous rotation 3 Kinematical refinement against 3D ED data 4 Dynamical refinement against 3D ED data 5 FIDEL fits 6 DFT calculations 8

Continuous electron diffraction data collection
A JavaScript controlling the goniometer speed was written. The script code is available at https://github.com/EvgenyGorelik/continuous_rotation. The script is performing the following steps: (i) a short delay is built in in order to give the operator a possibility to switch on the camera recording manually; (ii) then the beam is un-blanked and the goniometer starts rotating with a given speed to the  Figure S1. Technical data of all collected 3D ED datasets  Continuous rotation patterns can be seen as "linear" precession patterns. Different geometry of data collection may need an appropriate Lorentz correction. In this work we did not use any correction scheme.
The difference between static patters and continuous rotation may become crucial for beam sensitive crystals. CuPcCl 16 crystals were relatively stable, we did not have to make any significant precautions during the data collection. For static patterns, the amount of electron dose received by a crystal is proportional to the number of frames, which is, in turn, related to the total tilt range collected and the Acta Cryst. (2021). B77, https://doi.org/10.1107/S2052520621006806 Supporting information, sup-4 tilt increment, and the exposure time per frame. In our case, the largest tilt increment used was 0.5°, the exposure time per frame was 0.5 s.
For continuous rotation, the number of frames is inversely related to the effective tilt increment, which is determined by a combination of exposure and the rotation speed. In Figure 7 different values of effective tilt increment are plotted against the speed settings, spots on the red dashed line were obtained using 0.5 s exposure, on the green -0.5s, on the blue line 1 s. The total electron dose received by the crystal using the selected parameters is schematically represented by the size of the blue spots. We did not see any quality worsening for data sets recorded with high effective tilt increment. Therefore, the combination of high speed and low exposure will determine the strategy for beam sensitive materials. An obvious disadvantage of continuous rotation data acquisition is the absence of crystal tracking during the data collection, which sets high demands on the goniometer quality and limits on crystal size.

Figure S2 Interplay of parameters for continuous rotation as used in our experimental settings.
Kinematical refinement against 3D ED data Dynamical refinement against 3D ED data Figure S3 hk0 plane of the reciprocal volume reconstructed from 3D ED data using PETS2 (Prague, Czech Republic). Reference similarities S12 0 denote the limit of S12(l) as l approaches 0 over the full range of the experimental pattern, comparing the patterns including the background (unless the use of the background-corrected data is explicitly indicated by the superscript "bc").