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Crystal structure of copper perchlorophthalocyanine analysed by 3D electron diffraction
Author(s) -
Gorelik Tatiana E.,
Habermehl Stefan,
Shubin Aleksandr A.,
Gruene Tim,
Yoshida Kaname,
Oleynikov Peter,
Kaiser Ute,
Schmidt Martin U.
Publication year - 2021
Publication title -
acta crystallographica section b
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.604
H-Index - 33
ISSN - 2052-5206
DOI - 10.1107/s2052520621006806
Subject(s) - mosaicity , crystal structure , crystallography , electron diffraction , diffraction , materials science , powder diffraction , rietveld refinement , crystallographic point group , crystal (programming language) , x ray crystallography , chemistry , physics , optics , programming language , computer science
Copper perchlorophthalocyanine (CuPcCl 16 , CuC 32 N 8 Cl 16 , Pigment Green 7) is one of the commercially most important green pigments. The compound is a nanocrystalline fully insoluble powder. Its crystal structure was first addressed by electron diffraction in 1972 [Uyeda et al. (1972). J. Appl. Phys. 43 , 5181–5189]. Despite the commercial importance of the compound, the crystal structure remained undetermined until now. Using a special vacuum sublimation technique, micron‐sized crystals could be obtained. Three‐dimensional electron diffraction (3D ED) data were collected in two ways: (i) in static geometry using a combined stage‐tilt/beam‐tilt collection scheme and (ii) in continuous rotation mode. Both types of data allowed the crystal structure to be solved by direct methods. The structure was refined kinematically with anisotropic displacement parameters for all atoms. Due to the pronounced crystal mosaicity, a dynamic refinement was not feasible. The unit‐cell parameters were verified by Rietveld refinement from powder X‐ray diffraction data. The crystal structure was validated by many‐body dispersion density functional theory (DFT) calculations. CuPcCl 16 crystallizes in the space group C 2/ m ( Z = 2), with the molecules arranged in layers. The structure agrees with that proposed in 1972.