Single Crystal X-Ray Diffractometry

In X-ray diffraction (XRD) the interplanar spacing (d-spacing) of a crystal is used for identification and characterization purposes. In this case, the wavelength of the incident X-ray is known and measurement is made of the incident angle (Θ) at which constructive interference occurs. Solving Bragg’s Equation gives the d-spacing between the crystal lattice planes of atoms that produce the constructive interference. A given unknown crystal is expected to have many rational planes of atoms in its structure; therefore, the collection of “reflections” of all the planes can be used to uniquely identify an unknown crystal. In general, crystals with high symmetry (e.g. isometric system) tend to have relatively few atomic planes, whereas crystals with low symmetry (in the triclinic or monoclinic systems) tend to have a large number of possible atomic planes in their structures.


How it works

Single-crystal X-ray crystallography: A single crystal is need. It must be sufficiently large crystal (typically larger than 0.1 mm in all dimensions), pure in composition and regular in structure, with no significant internal imperfections such as cracks or twinning.

The crystal is exposed to an intense beam of X-rays, usually of a single wavelength (monochromatic X-rays), producing the regular pattern of reflections. The angles and intensities of diffracted X-rays are measured, with each compound having a unique diffraction pattern. As the crystal is gradually rotated, previous reflections disappear and new ones appear; the intensity of every spot is recorded at every orientation of the crystal. Multiple data sets may have to be collected, with each set covering slightly more than half a full rotation of the crystal and typically containing tens of thousands of reflections.

In the third step, these data are combined computationally with complementary chemical information to produce and refine a model of the arrangement of atoms within the crystal.