High-Energy X-Ray Structural Analysis Equipment

◆Equipment overview

General-purpose high-resolution structural analysis of organic and inorganic substances can be performed. This can be used for precise analysis of the electron density levels of functional materials.
Equipment Photo: Single crystal structural analysis device using a high-energy X-ray compatible semiconductor detector.

◆Features of the Equipment

This equipment can perform general-purpose, high-resolution structural analysis of organic and inorganic substances. This can be used for precise analysis of the electron density levels of functional materials. Equipped with a 1/4χ goniometer, it is possible to switch between the PILATUS３ X CdTe 1M semiconductor detector and a curved imaging plate.

・1/4χ Diffractometer
The diffractometer has three axes, ω, χ, and φ, which allows for comprehensive observation of the reciprocal space required for structural analysis.（IP: ２θmax < 145°; PILATUS: ２θmax < 65°）

・Detector
・High-energy X-ray Compatible Semiconductor Detector
This detector is a high-energy semiconductor detector which uses CdTe as the detection element. It is possible to read diffraction images at high speeds, as well as collect crystal structure analysis data in a very short time. Click here for detailed specifications.

・Large Curvature IP Camera
This detector has little selectivity for X-ray energy, but it has a wide dynamic range, and can observe a large area at once. It is used mainly for precision structure analysis, such as electron density distribution. Click here for detailed specifications.

・Control Software
The control software is manufactured by Rigaku, and is also used in the laboratory equipment, from the semiconductor to the large curvature IP camera, this software makes the collection of diffraction data possible.

◆Equipment accessories

The following accessories can be used with this system.
・Low-temperature Helium gas spray equipment (20 – 400 K)
・High-temperature Nitrogen gas spray equipment (300 – 800 K)
・Ultraviolet Irradiation Device
・Xenon light source
・High-pressure electric field application apparatus
・X-Ray pulse selector

◆Experiment / sample preparation

While taking measurements, laboratory equipment sample holders are available, including micromounts, loops or glass needles (with the height from the base about 20mm). The goniometer head can be held with a magnet or a φ3mm metal rod. When crystallinity deteriorates due to solvent desorption in air, it is possible to mount the sample at the beamline using a stereo microscope installed on the beamline.

◆Experimental procedure / precautions

Experiments on single crystal structure analysis can be performed using the same procedure as the laboratory equipment. The following are the procedures for general single structure crystal analysis experiments.

1)Mount the sample in the sample holder
Sample holders such as micromounts, loops and glass needles are commonly used in laboratory systems. (Height from the base is about 20mm)
2)Mount the sample holder on the diffractometer
3)Centering
Centering is performed on the φ and ω axes.
4)Evaluation of crystals by provisional measurements
The crystallization and diffraction strength are checked by measuring for a short time (several minutes).
5)Data measurement
Based on the outcome of the check measurements, the exposure time and X-ray intensity are decided and data measurements are completed. Generally, diffraction images are obtained every Δω＜1° within the range ω：0～180°at the φ：0，90,180,270°positions. The reading time of PILATUS is short, and shutterless measurement is performed. For 1 second exposure, the total reflection measurement is completed in approximately 12 minutes.
6)Diffraction Intensity Integration
Diffraction intensity is extracted from the diffraction image using the integration software introduced in the beamline. The available software is: Rapid Auto, CrysAlisPro(RIGAKU), APEX3(Bruker)
7)Structure Analysis
Structure analysis such as crystallography data as well as diffraction intensity data are obtained from performing integration processing. In general, it is recommended that users prepare software for structural analysis that is familiar to them, as analysis is generally carried out at universities and other facilities after the experiment.

◆Contact

杉本邦久（このメールアドレスはスパムボットから保護されています。閲覧するにはJavaScriptを有効にする必要があります。）
安田伸広（このメールアドレスはスパムボットから保護されています。閲覧するにはJavaScriptを有効にする必要があります。）
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◆List of representative treatises

"Observation of the Asphericity of 4f-electron Density and its Relation to the Magnetic Anisotropy Axis in Single-Molecule Magnets"
Gao Chen et al.
Nature Chemistry, 12, (2020) 213-219
DOI : 10.1038/s41557-019-0387-6

"X-ray Electron Density Investigation of Chemical Bonding in van der Waals Materials"
Kasai Hidetaka et al.
Nature Materials, 17, (2018) 249-252
DOI : 10.1038/s41563-017-0012-2

"A Linear Cobalt(II) Complex with Maximal Orbital Angular Momentum from a Non-Aufbau Ground State"
Bunting Philip C. et al.
Science, 362, (2018) eaat7319
DOI : 10.1126/science.aat7319

"Observation of Quadrupole Helix Chirality and its Domain Structure in DyFe₃(BO₃)₄"
Usui T. et al.
Nature Materials, 13, (2014) 611-618
DOI : 10.1038/NMAT3942

"Electronic Nematicity above the Structural and Superconducting Transition in BaFe₂(As_1-xP_x)₂"
Kasahara Shigeru et al.
Nature, 486, (2012) 382-385
DOI : 10.1038/nature11178

"Spin-Orbital Short-Range Order on a Honeycomb-Based Lattice"
Nakatsuji Satoru et al.
Science, 336, (2012) 559-563
DOI : 10.1126/science.1212154

"Photoactivation of a Nanoporous Crystal for On-Demand Guest Trapping and Conversion"
Sato Hiroshi et al.
Nature Materials, 9, (2010) 661-666
DOI : 10.1038/NMAT2808

"A Layered Ionic Crystal of Polar Li@C60 Superatoms"
Aoyagi Shinobu et al.
Nature Chemistry, 2, (2010) 678-683
DOI : 10.1038/NCHEM.698