Course syllabus

To give students the practical tools to collect data for, and understand, single crystal X-ray structure reporting.

The lectures you will find in this way:

Register for the Riga X-ray forum here: https://www.rigakuxrayforum.com. The instrument we use is a Synergy-R.

Then go to Rigaku School for Practical Crystallography January 2024 and view at least the following lectures:

Lecture 01 - Introduction
Lecture 03 - X-ray sample screening, strategy calculation and data collection
Lecture 05 - Integration
Lecture 06 - Data Finalization
Lecture 07 - Structure solution and refinement
Lecture 08 - Reporting and Checkcif

Then self-report in assignments, one for each lecture.

Whenever there are more than 1 student done we will have a structure seminar where you present the structure, how the practical work turned out, from selecting crystal to finalisation of the cif-file.

These are then the core learning goals:

1. Fundamental Concepts and Course Overview

• Explain the basic principles of single-crystal X-ray diffraction and its role in structural determination.
• Understand the workflow from crystal selection to final structure reporting.

2. Sample Screening, Strategy Calculation, and Data Collection 

• Assess the quality of single crystals for diffraction experiments.
• Set up and optimize data collection strategies based on crystal quality and symmetry.
• Operate an X-ray diffractometer to collect high-quality diffraction data.

3. Data Processing: Integration and Finalization

• Perform data integration, scaling, and corrections to produce high-quality datasets.
• Identify and address issues such as weak diffraction, twinning, or instrumental errors.
• Finalize datasets for structure solution by assessing data completeness and quality metrics.

4. Structure Solution and Refinement 

• Solve crystal structures using standard computational techniques such as direct methods or dual-space approaches.
• Refine crystal structures by applying appropriate constraints and restraints.
• Interpret key refinement parameters (e.g., R-factors, electron density maps, disorder modeling).

5. Structure Validation and Reporting 

• Use CheckCIF to validate structural data and identify potential errors or inconsistencies.
• Prepare comprehensive crystallographic reports, including CIF files, ORTEP representations, and refinement details.
• Understand the requirements for structure deposition in crystallographic databases (e.g., CCDC).

6. Application to Research

• Apply the learned techniques to collect, solve, and report a crystal structure relevant to the student's PhD research.
• Critically analyze diffraction results in relation to molecular structure and solid-state interactions.

Communicate crystallographic findings effectively in research papers, theses, and presentations.