Solid-State Hydration/Dehydration of Erythromycin A Investigated by ab Initio Powder X‑ray Diffraction Analysis: Stoichiometric and Nonstoichiometric Dehydrated Hydrate

• Published in: Crystal growth & design Vol. 13; no. 5; pp. 2060 - 2066
• Main Authors: Fujii, Kotaro, Aoki, Masahide, Uekusa, Hidehiro
• Format: Journal Article
• Language: English
• Published: Washington,DC American Chemical Society 01.05.2013
• Subjects: Condensed matter: structure, mechanical and thermal properties; Constant-composition solid-solid phase transformations: polymorphic, massive, and order-disorder; Cross-disciplinary physics: materials science; rheology; Exact sciences and technology; Growth from solutions; Materials science; Methods of crystal growth; physics of crystal growth; Phase diagrams and microstructures developed by solidification and solid-solid phase transformations; Physics; Structure of solids and liquids; crystallography; Structure of specific crystalline solids; Rietveld method; Crystalline phase; Crystal defects; Phase transformations; XRD; Erythromycin; Amorphous state; Heat treatments; Voids; Anhydrous compound; Solution structure; Humidity; Crystal growth from solutions; Ab initio calculations; Hydrates; Crystal structure
• ISSN: 1528-7483; 1528-7505
• DOI: 10.1021/cg400121u

The stable dihydrate crystalline phase (DH) of erythromycin A loses water upon heating to give the anhydrous phase I (AI). Further heating then results in a polymorphic transformation via the amorphous state (melt) to give another anhydrous phase II (AII). The anhydrous phases of AI and AII undergo hydration when increasing the humidity. The crystals of AI showed stoichiometric hydration to give DH, whereas the crystals of AII showed nonstoichiometric hydration to give the humidity dependent nonstoichiometric hydrate phase (NSH). The crystal structures of AI and AII were directly determined from powder X-ray diffraction data using the direct space strategy for the structure solution followed by Rietveld refinement. From the structural properties of AI and AII, aspects of the mechanism of the solid-state transformations of DH and the hydration behavior of AI and AII have been determined, and the importance of the hydrophilicity of the voids has been revealed.