*2.2. X-ray Structure Determination 2.2. X-ray Structure Determination*

*2.3. Powder X-ray Diffraction Experiments* 

Crystal of **ASZ**·1.5(**1,4-FIB**) was investigated on an Xcalibur, Eos diffractometer at 100 K (monochromated MoKα radiation with λ = 0.71073 Å). The structure was solved by the direct methods (SHELX program [23]) in the OLEX2 program package [24]. The carbon-bound H atom positions were calculated and included in the refinement in the 'riding' model approximation. Uiso(H) were set to 1.5Ueq(C) (for CH3 groups) or 1.2Ueq(C) (for CH2 and CH groups). The C–H bond lengths are 0.98 Å for CH3 groups, 0.99 Å for CH2 groups, and 0.95 Å for CH groups. Empirical absorption correction was applied in the CrysAlisPro [25] program. For crystallographic data and refinement parameters see Supplementary material (Table S3). Supplementary crystallographic data was deposited at Cambridge Crystallographic Data Centre (CCDC 1960975) and can be obtained free of charge via www.ccdc.cam.ac.uk/data\_request/cif. Crystal of **ASZ**·1.5(**1,4-FIB**) was investigated on an Xcalibur, Eos diffractometer at 100 K (monochromated MoKα radiation with λ = 0.71073 Å). The structure was solved by the direct methods (SHELX program [23]) in the OLEX2 program package [24]. The carbon-bound H atom positions were calculated and included in the refinement in the 'riding' model approximation. Uiso(H) were set to 1.5Ueq(C) (for CH<sup>3</sup> groups) or 1.2Ueq(C) (for CH<sup>2</sup> and CH groups). The C–H bond lengths are 0.98 Å for CH<sup>3</sup> groups, 0.99 Å for CH<sup>2</sup> groups, and 0.95 Å for CH groups. Empirical absorption correction was applied in the CrysAlisPro [25] program. For crystallographic data and refinement parameters see Supplementary material (Table S3). Supplementary crystallographic data was deposited at Cambridge Crystallographic Data Centre (CCDC 1960975) and can be obtained free of charge via www.ccdc.cam.ac.uk/data\_request/cif.

high-resolution diffractometer using monochromated CuKα (λ = 1.54184 Å) radiation.

The X-ray diffraction of powder samples was measured at room temperature on a D8 Discover
