Structural investigations of the XeF2–PtF5 system: crystal structures of [Xe2F3][PtF6]·XeF2, [Xe2F3][PtF6], and [XeF][PtF6]

Single-crystal X-ray diffraction Single-crystal X-ray diffraction data were collected at a temperature of 100 K on a Rigaku OD XtaLAB Synergy-S diffractometer equipped with a Dectris EIGER2 R CdTe 1M hybrid pixel array detector using microfocused Ag Kα radiation (λ = 0.56087 Å). CrysAlisPro software was employed for data processing, utilizing empirical and numerical absorption correction [1]. All crystal structures were solved using SUPERFLIP [2] and refined with SHELXL [3] within Olex2 software [4]. SCXRD-data folder: The supplied data comprise the raw diffraction images in .odeiger format, the associated data reduction and processing files, and the structure solution files. Raman Spectroscopy Low-temperature Raman spectra were measured at 100 K on a Bruker Senterra II confocal Raman microscope coupled with a Linkam LTS420 low-temperature stage, using a 785-nm emission line. The spectra were measured in the 50–1410 cm−1 range with a resolution of 1.5 cm−1. Prior to analysis, the samples were homogenized in an agate mortar within a glovebox and loaded into F2-passivated quartz capillaries (500 µm diameter), which were subsequently flame-sealed in a hydrogen–oxygen flame. Background subtraction using 3 iterations of concave rubber band correction with 64 baseline points was performed in Bruker Opus 8.7 software suite. Complete set of measurement parameters for each spectrum is given below: [Xe2F3][PtF6]·XeF2(mC120) (labelled as Xe3PtF11_mC) – 15 × 1000 µm aperture, 25 mW laser power, 20x objective. [Xe2F3][PtF6]·XeF2(oP120) (labelled as Xe3PtF11_oP) – 15 × 1000 µm aperture, 100 mW laser power, 20x objective. [Xe2F3][PtF6] (labelled as Xe2PtF9) – 15 × 1000 µm aperture, 100 mW laser power, 20x objective. [XeF][PtF6] (labelled as XePtF7) – 15 × 1000 µm aperture, 50 mW laser power, 20x objective. Raman-data folder: The subfolders labeled "processed" and "raw" contain, respectively, the final background subtracted Raman spectra and the spectra prior to background subtraction. All spectra are provided in the comma-delimited .dpt file format.