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Phase determination by wavelength-modulated diffraction. I. Centrosymmetric case.

T Koganezawa1, Y Yoshimura, N Nakamura

  • 1Faculty of Science and Engineering, Ritsumeikan University, Kusatsu, Shiga 525-8577, Japan.

Journal of Synchrotron Radiation
|August 7, 2001
PubMed
Summary
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Wavelength-modulated diffraction offers a new method for crystal structure phase determination. This technique successfully assigned correct phases to most reflections in a ferrocene derivative crystal, demonstrating its potential for crystallographic analysis.

Area of Science:

  • Crystallography
  • Materials Science
  • Physics

Background:

  • Crystal structure determination is crucial in materials science and chemistry.
  • Phase determination is a key challenge in X-ray crystallography.
  • Anomalous dispersion effects are utilized for phase retrieval.

Purpose of the Study:

  • To introduce and validate wavelength-modulated diffraction for phase determination.
  • To assess the accuracy and applicability of this novel method.
  • To explore its utility in centrosymmetric crystals.

Main Methods:

  • Wavelength-modulated diffraction was employed, varying X-ray wavelength near an absorption edge.
  • Intensity gradients (dI/dλ) of Bragg reflections were measured.
  • Measurements were performed on a ferrocene derivative crystal (C36H32O7Fe) using synchrotron radiation.

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Main Results:

  • The phase of the structure factor was successfully derived for a centrosymmetric crystal.
  • Out of 104 measured reflections, 101 were assigned correct phases.
  • The sign of the intensity gradient (dI/dλ) was sufficient for phase determination in this case.

Conclusions:

  • Wavelength-modulated diffraction is a viable method for crystal structure phase determination.
  • The technique shows high accuracy, particularly for centrosymmetric crystals.
  • Further investigation into error sources and application limits is warranted.