Ab initio structure determination of the hygroscopic anhydrous form of alpha-lactose by powder X-ray diffraction.

Acta Crystallogr B

Laboratoire de Dynamique et Structure des Matériaux Moléculaires (UMR CNRS 8024), UFR de Physique, Bâtiment P5, Université des Sciences et Technologies de Lille, 59655 Villeneuve d'Ascq Cédex, France.

Published: August 2004

Annealing of alpha-lactose monohydrate at 408 K yielded a mixture of this compound with hygroscopic anhydrous alpha-lactose. A powder X-ray diffraction pattern of this mixture was recorded at room temperature. The starting structural model of hygroscopic alpha-lactose was found by a Monte Carlo simulated-annealing method. The final structure was obtained through Rietveld refinements, with soft restraints on interatomic bond lengths and bond angles, and crystalline energy minimization to locate the H atoms of the hydroxy groups. The crystalline cohesion is achieved by networks of O-H...O hydrogen bonds that differ from those of the monohydrate phase. The width of the Bragg peaks is interpreted by a phenomenological microstructural approach in terms of isotropic size effects and anisotropic strain effects.

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http://dx.doi.org/10.1107/S0108768104014375DOI Listing

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