Self-assembled polynuclear lanthanide hydroxo complexes are important objects in the reticular chemistry approach to the design of various functional materials. Revealing their structure in the solid state and understanding the molecular mechanism of self-assembly in solution require a universal and reliable structural method. Pair distribution function (PDF) analysis is a powerful technique which enables structural insight for a wide range of crystalline and amorphous materials on the nanoscale, but commonly measurements are performed at synchrotron X-ray sources or on specially designed laboratory diffractometers. In the present paper, a standard Bruker D8 QUEST single-crystal X-ray diffractometer equipped with a micro-focus Mo tube and CMOS Photon III detector was adapted to measure PDF data of high quality with Q_max = 16.97 Å^–1 for solid and liquid samples. An improved data collection strategy and the original data reduction software FormagiX enable calibration and azimuthal full-frame integration of 2D frames, delivering reliable PDFs up to 80 Å with instrumental parameters Q_damp = 0.018 Å⁻¹ and Q_broad = 0.010 Å⁻¹. The effectiveness of the developed approach was demonstrated with reference samples and real-case studies of tetranuclear lanthanide hydroxocarboxylates in solid form and in solution.

中文翻译：

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使用实验室单晶 X 射线衍射仪快速可靠地采集 PDF 数据，用于研究固体形式和溶液中的多核镧系元素配合物

自组装多核镧系元素羟基配合物是网状化学方法中设计各种功能材料的重要对象。揭示它们在固态下的结构并了解溶液中自组装的分子机制需要一种通用且可靠的结构方法。对分布函数 (PDF) 分析是一种强大的技术，可以在纳米尺度上对各种晶体和非晶材料进行结构洞察，但通常在同步加速器 X 射线源或专门设计的实验室衍射仪上进行测量。在本文中，采用配备微焦点 Mo 管和 CMOS Photon III 探测器的标准 Bruker D8 QUEST 单晶 X 射线衍射仪测量高质量的 PDF 数据，Q对于固体和液体样品，_最大值= 16.97 Å ^{–1 。}改进的数据收集策略和原始数据缩减软件FormagiX可实现 2D 帧的校准和方位角全帧集成，提供高达 80 Å 的可靠 PDF，仪器参数Q_阻尼= 0.018 Å ^-1和Q_宽= 0.010 Å ^-1。所开发方法的有效性通过参考样品和固体形式和溶液中四核镧系羟基羧酸盐的实际案例研究得到证明。