Single-crystal X-ray diffractometry data for a sample of [Cu(HF₂)(pyrazine)₂]PF₆ collected on beamline I19-2 at Diamond Light Source

Single-crystal X-ray diffractometry data for a sample of [Cu(HF₂)(pyrazine)₂]PF₆.

These data were collected at Diamond Light Source, on beamline I19 (experiments hutch 2), on 2022-01-30, and are particularly useful for testing data reduction routines. They are known to produce good merging statistics and final structure refinement.

The sample was prepared as follows:
Ammonium hexafluorophosphate (NH₄PF₆) (0.310 g, 1.9 mmol), ammonium hydrogen difluoride ((NH₄)HF₂) (0.109 g, 1.9 mmol) and pyrazine (C₄H₄N₂) (0.300 g, 3.7 mmol) were dissolved in 5 mL of deionised water. The obtained colourless solution was slowly added to a blue solution of copper(II) nitrate prepared by dissolving copper(II) nitrate hemipentahydrate (Cu(NO₃)₂ · 2.5(H₂O)) (0.425 g, 1.8 mmol) in 5 mL of deionised water. The solutions were mixed in a plastic beaker at room temperature. The formation of blue crystals of [Cu(HF₂)(pyrazine)₂]PF₆ on the side of the beaker started after few seconds and continued for about 24 hours during which the sealed beaker was not moved.

The sample was measured at room temperature and the illuminating beam had a wavelength of 0.4859 Å (25.52 keV).

Beamline I19-2 at Diamond Light Source, a four-circle κ-geometry diffractometer (see [Kern 2019]) with an undulator source, is described in [Nowell 2012] but has since been upgraded to use a Dectris Eiger2 X 4M CdTe hybrid photon counting detector. The data are written in the NXmx variant of the NeXus format, and so include metadata with a functionally complete description of the diffractometer.

Inventory of data:

01_CuHF2pyz2PF6b_Phi.tar.xz
A single 1750-image 350° φ rotation scan from -175° to 175° with 0.2° rotation per image, an exposure time of 0.1 s per image, ω = -90°, κ = 0° and 2θ = 0°.

02_CuHF2pyz2PF6b_2T.tar.xz
A single 1750-image 350° φ rotation scan from -175° to 175° with 0.2° rotation per image, an exposure time of 0.1 s per image, ω = -90°, κ = 0° and 2θ = 20°.

03_CuHF2pyz2PF6b_P_O.tar.xz
Two sequential rotation scans:

CuHF2pyz2PF6b_P_O_01.nxs
A 1750-image 350° φ scan from -175° to 175° with ω = -90°, κ = 0° and 2θ = 0°.

CuHF2pyz2PF6b_P_O_02.nxs
A 600-image 120° ω scan from -125° to -5° with φ = -90°, κ = 45° and 2θ = 0°.

Both scans had 0.2° rotation per image and an exposure time of 0.1 s per image.

The same sample was used for all these measurements. Throughout, the sample-to-detector distance was 85 mm and the beam was attenuated to 0.2% of its full intensity.

For each rotation scan, the data comprise a single top-level NXmx-format NeXus file named .nxs, one or more image files named _00000n.h5, where n is a numeral, and a single detector metadata file named _meta.h5. The NeXus file contains an HDF5 virtual data set that links to the data in the image file(s), and several HDF5 external links to data in the detector metadata file.

For internal reference of Diamond Light Source staff, these data were collected as part of commissioning visit CM31144-1. Some file names and corresponding HDF5 link targets have been altered from their original names for consistency with the file contents.