Hydrogen-bonded salt cocrystals of xenon difluoride and protonated perfluoroamides

Single-crystal X-ray diffraction (SCXRD): Single-crystal and powder X-ray diffraction measurements were performed on a Rigaku OD XtaLAB Synergy-S Dualflex diffractometer equipped with a Dectris Eiger2 R CdTe 1M detector, PhotonJet-S microfocus Cu and Ag X-ray sources, and an Oxford Cryosystems 800 Series Cryostream. All datasets were processed with empirical and numerical absorption corrections using CrysAlisPro software. [1] Crystal structures were solved by the charge flipping method using olex2.solve, [2] whereas (CF3CONH2)2H[AsF6] was solved with SHELXT, [3] and subsequently refined using SHELXL [4] within Olex2. [5] SCXRD data folder: The folder contains the raw diffraction images in the .odeiger file format, the relevant data reduction and processing files, and the structure solution files. Powder X-ray diffraction (PXRD): The powder diffractogram of CF3C(OH)NH2[AsF6]∙XeF2 was measured at 100 K by mounting large amount of crystallites on the tip of a MiTeGen MicroLoop using Fomblin oil (Z25, SynQuest). Gandolfi movements were employed to enhance the random orientation of the crystallites. A measurement consisted of six frames, each with an exposure time of 300 s, with the detector positioned 90 mm away from the sample. The calculated powder diffractogram of CF3C(OH)NH2[AsF6]⋅XeF2 was obtained from Mercury 2025.2.0. [6] (0.56087 Å, 2θ step = 0.01°, fwhm = 0.1). PXRD data folder: The supplied dataset consists of extracted powder diffractogram in the tab separated .dat file format, the raw diffraction images in the .odeiger file format and the calculated powder diffractogram of CF3C(OH)NH2[AsF6]⋅XeF2. Raman spectroscopy: Raman spectra were measured using a Horiba Jobin Yvon Labram-HR spectrometer coupled with an Olympus BXFM-ILHS microscope, employing either a red or a green laser with 633 nm and 532 nm emission lines, respectively. The typical spectral resolution was 4 cm−1. The slit size was 100 microns, whereas the hole size was 1000 microns. The Raman spectra of all compounds were recorded directly on the aluminium trough, cooled by a cold nitrogen stream, which was also used to mount the crystals for X-ray diffraction. The background subtraction was performed in the Bruker OPUS 8.7. Build: 8, 7, 41 [20220611 x64] software suite using concave rubberband correction (15 iterations, 50 baseline points). CF3CONH2 : 633 nm, 24 mW nominal laser power, 10x objective, recorded at 183 K. C2F5CONH2 : 532 nm, 40 mW nominal laser power, 10x objective, recorded at 183 K. C3F7CONH2 : 633 nm, 24 mW nominal laser power, 10x objective, recorded at 183 K. CF3C(OH)NH2[AsF6]: 633 nm, 24 mW nominal laser power, 10x objective, recorded at 173 K. C2F5C(OH)NH2[AsF6]: 633 nm, 24 mW nominal laser power, 10x objective, recorded at 223 K. C3F7C(OH)NH2[AsF6]: 633 nm, 24 mW nominal laser power, 10x objective, recorded at 173 K. CF3C(OH)NH2[AsF6]⋅XeF2: 633 nm, 24 mW nominal laser power, 10x objective, recorded at 183 K. C2F5C(OH)NH2[AsF6]⋅XeF2: 633 nm, 24 mW nominal laser power, 10x objective, recorded at 183 K. C3F7C(OH)NH2[AsF6]⋅XeF2: 633 nm, 24 mW nominal laser power, 10x objective, recorded at 180 K. Raman data folder: The supplied dataset consists of raw and background-subtracted Raman spectra in the tab-separated .txt files, together with the specifications for background substraction.