Published in

International Union of Crystallography, Acta Crystallographica Section B: Structural Science, Crystal Engineering and Materials, 4(75), p. 657-673, 2019

DOI: 10.1107/s2052520619006681

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The role of multiple observations in small-molecule single-crystal service X-ray structure determination

Journal article published in 2019 by Alice E. Williams, Amber L. Thompson ORCID, David J. Watkin ORCID
This paper was not found in any repository, but could be made available legally by the author.
This paper was not found in any repository, but could be made available legally by the author.

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Data provided by SHERPA/RoMEO

Abstract

In order to gain a better understanding of how to improve the quality of small-molecule single-crystal X-ray diffraction data achievable in a finite time, a study was carried out to investigate the effect of varying the multiplicity, acquisition time, detector binning, maximum resolution and completeness. The results suggest that, unless there are strong arguments for a different strategy, a good routine procedure might be to optimize the conditions necessary to get the best data from single scans, and then choose a multiplicity of observations (MoO) to utilize the available time fully. Different strategies may be required if the crystal is highly absorbing, is larger than the incident beam, is enclosed in a capillary tube or is unusual in some other way. The signal-to-noise ratio should be used with care, as collecting data for longer or at higher multiplicity appears to give a systematic underestimate of the intensity uncertainties. Further, the results demonstrate that including poor-quality data in a refinement may degrade the result and, in the general case, the accidental omission of reflections has a very small impact on the refinement as long as they are omitted at random. Systematic omission of reflections needs a convincing procedural justification.