Theoretical and practical single crystal X-ray structure determination

The aim of the course is to give an introduction to theoretical and practical single crystal X-ray diffraction structure determination. Solid materials are of utmost relevance in a wide range of application areas covering the full breadth of chemical science. Examples of active research at the Department of Chemistry include pharmaceutically active compounds, coordination compounds, homogeneous organometallic catalysts, inorganic and inorganic-organic hybrid materials for catalysis and sorption processes.

The most important initial characterization after synthesis of a new compound is the attempt to obtain information about the structure of the material on an atomic level. Solid materials are divided into two groups, crystalline and amorphous. Crystalline substances have a periodic and regular arrangement of atoms. Their structure can be determined from diffraction data, performed either on single crystals or microcrystalline powders. In the case of large single crystals, crystal structure determination has become a rapid and routine process in the majority of cases.

The main purpose of this course is to provide the participant with the necessary theoretical and practical background knowledge and practical experience to be able to successfully determine the crystal structure from single crystal X-ray diffraction data and be able to present this knowledge in scientific dissemination. To achieve this aim, the course consists of three parts:

1. Theory

The necessary theoretical background about crystal structures, X-ray diffraction and the process of structure determination using diffraction-based techniques is taught in a block course.

2. Exercises

Participants will receive a demonstration of how single crystal X-ray diffraction experiments are performed in practice. Participants will be trained in software used for structure determination and presentation of results. Introduction to the software will be part of the block course, the participants will practice a full structure determination using a provided dataset on their own. There will be a couple of joint sessions to present their results and address questions and problems they may have encountered.

3. Exam that includes performing an actual crystal structure determination

On completion of the course the student should have the following learning outcomes defined in terms of knowledge, skills and general competence:

Knowledge

The student is able to

• Explain the principles of X-ray diffraction and the information contained in diffraction patterns.
• Understand and describe the structure of crystalline materials.
• Discuss the principles and steps involved in single crystal structure determinations.

Skills

The student is able to

• Perform (in principle) single crystal X-ray diffraction experiments.
• Use typical software to analyze and present the data collected in a single crystal X-ray diffraction experiment.
• Select the appropriate approach for structure solution and refinement (i.e. perform a single crystal structure determination) and summarize it in writing.
• Present crystal structures in words and figures and identify and describe relevant structural details that merit emphasis.
• Prepare figures and tables for presentation of single crystal structures.
• Read and edit electronic files required for electronic dissemination (e.g. submission to databases).
• Use the Cambridge Structural Database for search and comparison of compounds and structures.

General competence

The student is able to

• Convey the central content of the subject both in written and verbal form and by use of expressions characteristic for the subject (e.g. summary texts on how the structure determination was performed, structure drawings and tables).
• Work together in groups and perform practical tasks (software).
• Interpret information about the structure of compounds and materials.
• Write summaries of relevant information.
• Identify and assimilate relevant knowledge from teaching material through lectures, group work and on their own.