Single-Crystal X-Ray Diffraction of Compounds 1 and 5

Crystals of compounds 1 and 5 were obtained by slow evaporation at 4 °C. A suitable crystal was selected for each of them, mounted on a nylon loop and fixed with oil. Then, X-ray diffraction and crystallographic data were collected at room temperature using redundant ω scans on a Rigaku XtaLabPro single-crystal diffractometer using microfocus Mo Kα radiation and an HPAD PILATUS3 R 200K detector.
Using Olex2 [50 (link)], the structures were readily solved by intrinsic phasing methods (SHELXT [51 (link)]) and by full-matrix least-squares methods on F2 using SHELXL [52 (link)]. The nonhydrogen atoms were refined anisotropically, and most of the hydrogen atoms were identified in difference maps and were treated as riding on their parent atoms.
For each structure, the Flack parameter [53 (link)] was refined. The determination of the absolute structure was confirmed by using Bayesian statistics on Bijvoet differences [54 (link)] based on the Olex2 results.
All the molecular graphics presented here were computed with Mercury 2020.3.0 [55 (link)].
Crystallographic data for the two structures (1 and 5) have been deposited in the Cambridge Crystallographic Data Centre database (the deposition numbers are CCDC 2085749 and CCDC 2085750, respectively). Copies of the data can be obtained free of charge from the CCDC at www.ccdc.cam.ac.uk (accessed on 7 July 2021).