Mechanical amorphization of three chitosan samples with high, medium, and low molecular weight was studied. It is shown that there are no significant differences between the course of amorphization process in a planetary ball mill of chitosan with different molecular weights, and the maximum degree of amorphization was achieved in 600 s of high intensity mechanical action. Specific energy consumption was 28 kJ/g, being comparable to power consumption for amorphization of cellulose determined previously (29 kJ/g) and 5–7-fold higher than that for amorphization of starch (4–6 kJ/g). Different techniques for determining the crystallinity index (CrI) of chitosan (analysis of the X-ray diffraction (XRD) data, the peak height method, the amorphous standard method, peak deconvolution, and full-profile Rietveld analysis) were compared. The peak height method is characterized by a broader working range but provides deviated CrI values. The peak deconvolution method (with the amorphous Voigt function) makes it possible to calculate the crystallinity index of chitosan with greater accuracy, but the analysis becomes more difficult with samples subjected to mechanical processing. In order to refine the structure and calculation of CrI by the Rietveld method, an attempt to optimize the structure file by the density functional theory (DFT) method was performed. The averaged profile of amorphous chitosan approximated by an eighth-order Fourier model improved the correctness of the description of the amorphous contribution for XRD data processing. The proposed equation may be used as a universal standard model of amorphous chitosan to determine the crystallinity index both for the amorphous standard method and for peak deconvolution of XRD patterns for arbitrary chitosan samples.

There are many methods that can be used to incorporate concepts of crystallography into the learning experiences of students, whether they are in elementary school, at university or part of the public at large. It is not always critical that those who teach crystallography have immediate access to diffraction equipment to be able to introduce the concepts of symmetry, packing or molecular structure in an age- and audience-appropriate manner. Crystallography can be used as a tool for teaching general chemistry concepts as well as general research techniques without ever having a student determine a crystal structure. Thus, methods for younger students to perform crystal growth experiments of simple inorganic salts, organic compounds and even metals are presented. For settings where crystallographic instrumentation is accessible (proximally or remotely), students can be involved in all steps of the process, from crystal growth, to data collection, through structure solution and refinement, to final publication. Several approaches based on the presentations in the MS92 Microsymposium at the IUCr 23rd Congress and General Assembly are reported. The topics cover methods for introducing crystallography to undergraduate students as part of a core chemistry curriculum; a successful short-course workshop intended to bootstrap researchers who rely on crystallography for their work; and efforts to bring crystallography to secondary school children and non-science majors. In addition to these workshops, demonstrations and long-format courses, open-format crystallographic databases and three-dimensional printed models as tools that can be used to excite target audiences and inspire them to pursue a deeper understanding of crystallography are described.

The present study delivers a computational approach for the understanding of the mechanism of phase transitions between polymorphs of small organic molecules.

The existence of a new polymorph of metacetamol together with its properties are reported for the first time.

Two polymorphs of tolazamide, N-[(azepan-1-ylamino)carbonyl]-4-methylbenzenesulfonamide, a sulfonylurea anti-diabetic drug, have different densities and molecular packings. Polymorph II converts into polymorph I in the solid state on heating or via recrystallization if solvent-assisted. The effect of pressure on the two forms and the possibility of a transformation to a denser form on compression have been studied. No phase transitions have been observed in either of the forms in a pentane–isopentane mixture (when no recrystallization is possible). Polymorph II recrystallized partly into a denser polymorph I in methanol at 0.1 GPa, but the transformation stopped at an early stage. Solid state DFT calculations of the two forms as well as conformational landscape investigation in the gas phase were used to rationalize this result. The anisotropic pressure-induced strain of the two polymorphs has been compared in relation to changes in the hydrogen bond geometry and the behavior of stacking interactions.

High-pressure chemistry of organic compounds is a hot topic of modern chemistry. In this work, basic computational concepts for high-pressure phase transition studies in molecular crystals are described, showing their advantages and disadvantages. The interconnection of experimental and computational methods is highlighted, showing the importance of energy calculations in this field. Based on our deep understanding of methods’ limitations, we suggested the most convenient scheme for the computational study of high-pressure crystal structure changes. Finally, challenges and possible ways for progress in high-pressure phase transitions research of organic compounds are briefly discussed.