Electron crystallography on polymorphic organics

Abstract

Abstract Organic materials, such as non-linear optical active compounds (1-(2-furyl)-3-(4-aminophenyl)-2-propene-1-one (FBAPPO) and 1-(2-furyl)-3-(4-benzamidophenyl)-2-propene-1-one (FAPPO)), polymeric materials like the metal coordinated polyelectrolyte (Fe(II) [ditopic bis-terpyridin] (MEPE)) or polymorphic materials (e.g. Cu-phthalocyanine), which do not crystallize big enough for single crystal x-ray structure analysis have been investigated by electron diffraction (ED) at 100 and 300 kV acceleration voltage. Sample preparation (direct crystallization, ultra sonication, ultra microtomy), diffraction strategies (selected area diffraction, nano diffraction, use of double-tilt rotation holder), data collection and data processing as well as structure solution strategies have been chosen dependent on the different requirements of the compounds under investigation. Structure analysis was carried out by simulation using ab initio quantum-mechanical methods like density functional theory (DFT), semi-empirical approach (MNDO/AM1/PM3) and force field packing energy calculations (DREIDING). The structure models resulting from simulation were refined kinematically as rigid bodies. Subsequently, refinements by multi-slice least squares (MSLS) procedures taking dynamical scattering into account were performed. The described combination of different methods which was used successfully on crystallizable materials is also adaptable to insoluble organic materials (e.g. pigments) and polymorphic systems.