Crystal-structure refinement by profile fitting and least-squares analysis of powder diffractometer data

Abstract
The refinement of crystal structures using X-ray powder data in a two-stage method is described. (1) The integrated intensities of the individual reflections are derived by a profile fitting method in which the profile shapes are accurately defined using an experimentally determined instrument function and the sum of Lorentzian curves. (2) These values are then used in a powder least-squares refinement for structure determination. The results obtained with three simple structures (silicon, quartz and corundum) gave R(Bragg) values of 0.7 to 2.5%. The necessity of correcting for preferred orientation and the importance of proper specimen preparation are also discussed.

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