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Quick and robust PDF data acquisition using a laboratory single-crystal X-ray diffractometer for study of polynuclear lanthanide complexes in solid form and in solution

DOI: 10.1107/S1600576722005878 DOI Help

Authors: Dmitry Tsymbarenko (Lomonosov Moscow State University) , Dimitry Grebenyuk (Lomonosov Moscow State University) , Maria Burlakova (Lomonosov Moscow State University) , Mirijam Zobel (RWTH Aachen University)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Journal Of Applied Crystallography , VOL 55

State: Published (Approved)
Published: August 2022

Abstract: 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 Qmax = 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 Qdamp = 0.018 Å−1 and Qbroad = 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.

Journal Keywords: total X-ray scattering; pair distribution function; polynuclear lanthanide complexes

Subject Areas: Technique Development, Chemistry

Instruments: I15-1-X-ray Pair Distribution Function (XPDF)

Added On: 01/08/2022 09:11

Discipline Tags:

Technique Development - Chemistry Chemistry

Technical Tags:

Scattering Pair Distribution Function (PDF)