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

评价了一种以成像板为二维探测器的单晶x射线衍射仪适用于金属配合物的结构分析。利用IP x射线衍射仪测量了多种金属配合物单晶的x射线衍射数据，并对其进行了结构分析。为了与这些结果相比较，我们还利用典型的单晶结构分析仪器——4圆x射线衍射仪对其中的10种金属配合物进行了测量。IP x射线衍射仪的分析结果令人满意。研制了一种能与IP x射线衍射仪安装在一起的金刚石砧池（DAC）作为高压仪器。这是一个40毫米φ的DAC，比典型的单晶衍射DAC更泡沫。同时研制了适用于40 mmφDAC和IP x射线衍射仪的测角头。研制了高精度垫片孔钻床和各种夹具，可对DAC中极小的单晶进行精密加工。在测角仪周围重建了照明系统、光束阻挡器和准直器，以便将DAC安装在IP X-my衍射仪上。检查了装有DAC的测角仪的运动，确认运动中没有发生碰撞和其他任何问题，但在检查过程中，由于DAC的重量，观察到测角仪头部发生了扭转，因此对测角仪头部进行了重建以加强。研究和发展了在IP x射线衍射仪上测量DAC单晶的方法和技术。

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.