Structure determination of the 1/1 alpha/beta mixed lactose by X-ray powder diffraction

Acta Crystallogr B. 2005 Aug;61(Pt 4):455-63. doi: 10.1107/S0108768105017064. Epub 2005 Jul 19.

Abstract

The mixed form of alpha/beta lactose was obtained by heating amorphous alpha-lactose at 443 K. NMR spectroscopy determined the stoichiometry of this mixed compound to be 1/1. The X-ray powder diffraction pattern was recorded at room temperature with a sensitive curved detector (CPS 120). The structure was solved by real-space methods (simulated annealing) followed by Rietveld refinements with soft constraints on bond lengths and bond angles. The H atoms of the hydroxyl groups were localized by minimization of the crystalline energy. The cell of 1/1 alpha/beta lactose is triclinic with the space group P1 and contains two molecules (one molecule of each anomer). The crystalline cohesion is achieved by networks of O-H...O hydrogen bonds. The width of the Bragg peaks is interpreted through a microstructural approach in terms of isotropic strain effects and anisotropic size effects.

MeSH terms

  • Carbohydrate Conformation
  • Hydrogen Bonding
  • Lactose / chemistry*
  • Models, Molecular
  • Powder Diffraction*
  • X-Ray Diffraction

Substances

  • Lactose