Trial production of single-crystal X-ray diffractometer with 2D detector for high-pressure crystallography

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A single-crystal X-ray diffractometer with Imaging Plate(IP) as a two dimensional detector was assessed suitable for structure analysis of metal complexes. X-ray diffraction data were measured for a number of single-crystals of various metal complexes using the IP X-ray diffractometer, and their structure analyses were performed To compare with these results, ten of their metal complexes were also measured by using a 4-circle X-ray diffractometer, which is a typical one for the single-crystal structure analysis. The results of the analyses from the IP X-ray diffractometer were satisfactory.A diamond-anvil-cell (DAC) being able to be mount with the IP X-ray diffractometer was developed as a high-pressure apparatus. That is a 40 mmφ DAC, which is lather than a typical DAC for single-crystal diffraction. A goniometer-head was also developed suitable for the 40 mmφDAC and the IP X-ray diffractometer.A high precise drilling machine for gasket hole and various jigs were manufactured to precisely manipulate very small single crystals in the DAC.A lighting system, a beam-stopper, and collimaters around the goniometer were rebuilt to mount the DAC on the IP X-my diffractometer.Movement of the goniometer with DAC was checked It is confirmed that the collision and any other trouble were not happened in the movement As a torsion of the goniometer-head was, however, observed due to the weight of the DAC in the check process, the goniometer-head was rebuilt to strengthen it.Measurement procedures and technique were studied and developed for the single crystal in the DAC on the IP X-ray diffractometer.