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Languages: English
Types: Doctoral thesis
This thesis comprises the results of research on various aspects of solid inclusion compounds and other organic materials. Chapter 1 is an introduction to solid-state inclusion compounds, in particular describing the main characteristics of urea inclusion compounds and thiourea inclusion compounds. The experimental techniques utilized during the research are described in Chapter 2. These techniques include X-ray diffraction techniques (single crystal X-ray diffraction, powder X-ray diffraction and the characteristics of synchrotron radiation) and thermal analysis techniques (differential scanning calorimetry and thermogravimetric analysis). In Chapter 3, the main focus concerns studies of the solid-state properties of a special type of non-conventional urea inclusion compound formed with a,co-diaminoalkane guest molecules, and also incorporating methanol molecules within the structure. The present work is focused primarily on the stability of these materials, and the evolution of structural phases formed upon decomposition as function of time. Novel X-ray birefringence and X-ray dichroism investigations carried out at the Diamond Light Source (UK) on different thiourea inclusion compounds (1-bromoadamantane/thiourea inclusion compound, 2-bromoadamantane/thiourea inclusion compound and bromocyclohexane/thiourea inclusion compound, which has an order-disorder phase transition at low temperature) are reported in Chapter 4, where pioneering X-ray dichroism and X-ray birefringence measurements in organic compounds have proved to serve as a sensitive probe of changes in molecular orientation at order-disorder phase transitions. Chapter 5 is aimed at broadening the understanding of polymorphism and chemical reactivity of oxalyl dihydrazide at high temperatures using time-resolved powder X-ray diffraction data recorded at the Daresbury SRS (UK). Chapter 6 reports a powder X-ray diffraction study of the solid-state dehydration process of r-butylammonium acetate monohydrate, and the structural consequences of the dehydration process.
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    • Chapter 1 - Introduction
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