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:<br> 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: <strong><code>01_CuHF2pyz2PF6b_Phi.tar.xz</code></strong><br> 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°. <strong><code>02_CuHF2pyz2PF6b_2T.tar.xz</code></strong><br> 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°. <strong><code>03_CuHF2pyz2PF6b_P_O.tar.xz</code></strong><br> Two sequential rotation scans: <strong><code>CuHF2pyz2PF6b_P_O_01.nxs</code></strong><br> A 1750-image 350° φ scan from -175° to 175° with ω = -90°, κ = 0° and 2θ = 0°. <strong><code>CuHF2pyz2PF6b_P_O_02.nxs</code></strong><br> 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 <code>&lt;filename&gt;.nxs</code>, one or more image files named <code>&lt;filename&gt;_00000n.h5</code>, where <code>n</code> is a numeral, and a single detector metadata file named <code>&lt;filename&gt;_meta.h5</code>. 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.[Cu(HF₂)(pyrazine)₂]PF₆样品的单晶X射线衍射术（Single-crystal X-ray diffractometry）数据。本数据集采集于钻石光源（Diamond Light Source）的I19光束线（实验舱2），采集日期为2022年1月30日，尤其适用于数据还原程序的测试，其具备优异的合并统计结果与最终结构精修效果。 样品制备流程如下：将六氟磷酸铵（NH₄PF₆，0.310 g，1.9 mmol）、氟化氢二铵((NH₄)HF₂，0.109 g，1.9 mmol)与吡嗪（pyrazine，C₄H₄N₂，0.300 g，3.7 mmol）溶于5 mL去离子水中。将所得无色溶液缓慢加入由半五水合硝酸铜(II)（Cu(NO₃)₂·2.5H₂O，0.425 g，1.8 mmol）溶于5 mL去离子水配制的蓝色硝酸铜(II)溶液中。混合液置于塑料烧杯中于室温下静置，数秒后烧杯内壁即开始析出[Cu(HF₂)(吡嗪)₂]PF₆蓝色晶体，析出过程持续约24小时，期间密封烧杯静置不动。 样品在室温下进行测试，入射光束波长为0.4859 Å（对应能量25.52 keV）。钻石光源的I19-2光束线采用四圆κ几何构型衍射仪（详见[Kern 2019]），配备波荡器光源（undulator source），其原始设计参见[Nowell 2012]，后续已升级为使用Dectris Eiger2 X 4M CdTe混合光子计数探测器（Dectris Eiger2 X 4M CdTe hybrid photon counting detector）。本数据集采用NeXus格式（NeXus format）的NXmx变体（NXmx variant）存储，包含完整描述衍射仪的元数据。 数据文件清单如下： <strong><code>01_CuHF2pyz2PF6b_Phi.tar.xz</code></strong>：包含一组1750幅图像的350°φ旋转扫描（φ rotation scan）数据，扫描范围为-175°至175°，每幅图像对应0.2°旋转，单幅图像曝光时间0.1 s，实验参数为ω=-90°、κ=0°、2θ=0°。 <strong><code>02_CuHF2pyz2PF6b_2T.tar.xz</code></strong>：包含一组1750幅图像的350°φ旋转扫描数据，扫描范围为-175°至175°，每幅图像对应0.2°旋转，单幅图像曝光时间0.1 s，实验参数为ω=-90°、κ=0°、2θ=20°。 <strong><code>03_CuHF2pyz2PF6b_P_O.tar.xz</code></strong>：包含两组连续旋转扫描： <strong><code>CuHF2pyz2PF6b_P_O_01.nxs</code></strong>：1750幅图像的350°φ扫描数据，扫描范围为-175°至175°，实验参数为ω=-90°、κ=0°、2θ=0°。 <strong><code>CuHF2pyz2PF6b_P_O_02.nxs</code></strong>：600幅图像的120°ω扫描（ω rotation scan）数据，扫描范围为-125°至-5°，实验参数为φ=-90°、κ=45°、2θ=0°。 两组扫描均采用每幅图像对应0.2°旋转，单幅图像曝光时间0.1 s。 所有测试均使用同一批次样品，全程保持样品-探测器距离为85 mm，入射光束强度衰减至原强度的0.2%。 每组旋转扫描的数据包含：单个顶层NXmx格式NeXus文件（命名为<code>&lt;filename&gt;.nxs</code>）、一个或多个命名为<code>&lt;filename&gt;_00000n.h5</code>的图像文件（其中<code>n</code>为数字），以及一个命名为<code>&lt;filename&gt;_meta.h5</code>的探测器元数据文件。NeXus文件包含指向图像文件数据的HDF5格式（HDF5 format）虚拟数据集，以及若干指向探测器元数据文件的HDF5外部链接。 对于钻石光源内部工作人员而言，本数据集属于调试到访项目CM31144-1的一部分。为确保与文件内容一致，部分文件名及对应的HDF5链接目标已从原始名称进行了调整。