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.