Dualflex

Single-crystal X-ray diffraction data were collected at 100 K on an XtaLAB Synergy, Dualflex, Pilatus 300 K diffractometer apparatus (Rigaku Corporation, Tokyo, Japan) for compound 11. Using Olex2 [41 (link)], the structure was solved with the SHELXT [42 (link)] structure solution program using Intrinsic Phasing and refined with the SHELXL [43 (link)] refinement package using least-squares minimization. The CIF file containing full crystallographic data for compound 11 (CCDC 2278736) can be obtained free of charge from The Cambridge Crystallographic Data Centre via http://www.ccdc.cam.ac.uk/structures (accessed on 11 July 2023).

The crystallographic data were measured on a Bruker SMART APEX II CCD single crystal diffractometer with MoKα radiation (1–7, 9, 10, and 12–14) and an XtaLAB Synergy, Dualflex, HyPix diffractometer from Rigaku with CuKα radiation (11). The data were refined by SHELXL,^[28] and all non‐proton coordinate values and anisotropic temperature factors were refined by the full‐matrix least‐squares method. All proton positions in the structure were determined by theoretical calculation

Crystallization of suitable crystals for single-crystal X-ray analysis was not an easy task due to the tendency of 4B8M to form syrup-like amorphous phase or ‘twinned’ crystals. Finally, after many attempts, acceptable quality single crystals were grown via slow evaporation of a glacial acetic acid.
X-ray data were collected on a Rigaku OD XtaLAB Synergy, Dualflex, Pilatus diffractometer using graphite monochromated CuKα radiation (λ = 1.54158 Å) at a temperature of 100 K, using Crysalis, structure determination and refinement by Olex2 [118 (link)]. The structure was solved with the XT [119 (link)] structure solution program using intrinsic phasing and refined with the XL [120 (link)] refinement package using least-squares minimization. A CIF file containing complete information of the studied structure was deposited with CCDC, deposition number 2158219 is freely available upon request from the Director, CCDC, 12 Union Road, Cambridge CB2 1EZ, UK (Fax: + 44-1223-336033; e-mail: deposit@ccdc.cam.ac.uk).
All molecular interactions in the crystals of 4B8M and YEPVIZ were identified by the PLATON [121 (link)] and Mercury [116 (link)] programs.