The crystal structures of the title compound were determined by means of single-crystal X-ray diffraction at a number of different temperatures (110, 150, 190, 250, 290, 350), using tailor-made, theoretically calculated aspherical atomic scattering factors.
The dataset consists of 6 zip files, each one containing:
a) the final structure model obtained from X-ray diffraction data at given temperature in crystallographic format (a .cif file)
and
b) the final set of atomic scattering factors tabularized in a .tscb file.
The set of two files together is necessary to automatically repeat the crystal structure refinement by uploading them into Olex2.
The list of files:
110.zip : structure model and scattering factors determined at 110K
150.zip : structure model and scattering factors determined at 150K
190.zip : structure model and scattering factors determined at 190K
250.zip : structure model and scattering factors determined at 250K
290.zip : structure model and scattering factors determined at 290K
350.zip : structure model and scattering factors determined at 350K
##Structure solution and refinement
The determination of unit cell, data reduction and absorption correction were performed in software provided with the diffractometer - using CrysAlis PRO Version 1.171.39.43d. The structure solution and refinement was performed within Olex2 graphical environment. For the solution ShelXT with intrinsic phasing was used. For refinement ShelXL with least squares. All hydrogen atoms were located in the difference map and refined freely – in cases where free refinement was not possible, the hydrogens were refined as riding on their respective heavy atom.
Refinement was performed using NoSpherA2, an implementation of NOn-SPHERical Atom-form-factors in Olex2. (F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021) NoSpherA2 implementation of HAR makes use of tailor-made aspherical atomic form factors calculated on-the-fly from a Hirshfeld-partitioned electron density (ED). The ED was calculated for a single molecule of 1,3-di-acetylpyrene from a gaussian basis set single determinant SCF wavefunction with DFT using the following options:
SOFTWARE: ORCA 5.0
PARTITIONING: NoSpherA2
METHOD: B3LYP
BASIS SET: 6-31G(d,p)
CHARGE: 0
MULTIPLICITY: 1
##Model description
1,3-di-acetylpyrene "beta" polymorph crystallizes in P21/c space group with one molecule of 1,3-di-acetylpyrene in the asymmetric unit.
