A Solid-State Dehydration Process in an Organic Material Associated with Substantial Hydrogen-Bond Reorganization, Investigated by Powder X-ray Diffraction

Solid tert-butylammonium acetate monohydrate undergoes a facile solid-state dehydration process under ambient conditions, in which single crystals of the monohydrate phase transform to a microcrystalline powder of an anhydrous product phase. The structural properties of the anhydrous phase have been determined directly from powder X-ray diffraction data, employing the direct-space genetic algorithm technique for structure solution followed by Rietveld refinement, allowing rationalization of the structural changes associated with the dehydration process. The dehydration process is associated with substantial reorganization of the hydrogen bonding arrangement, although one component of the hydrogen-bonding scheme is actually preserved in the transformation.

固态醋酸叔丁基铵一水合物可在环境条件下顺利发生固态脱水过程，其一水合物相的单晶会转变为无水产物相的微晶粉末。研究人员通过粉末X射线衍射数据直接解析得到该无水相的结构性质，采用直接空间遗传算法进行结构解析，随后辅以里特维尔德（Rietveld）精修，从而阐明了与脱水过程相关的结构变化。该脱水过程涉及氢键排布的大幅重构，尽管在该转变过程中氢键作用模式的一组组分得以保留。