E13 – Small Molecule Single Crystal X-Ray Crystallography in Structural Chemistry

Small Molecule Single Crystal X-Ray Crystallography in Structural Chemistry

NEW Half-Day Course, E13-34, Wednesday, November 20th, 1:00pm – 4:30pm

 Dr. Nina C. Gonnella, Boehringer Ingelheim, Ridgefield, CT

Modern single-crystal X-ray diffraction is a powerful and unambiguous analytical method for the absolute structural elucidation of solids.  This course will provide a basic overview of X-ray crystallography as it applies to structure elucidation of small organic molecules. Basic principles of X-ray crystallography will be presented.  Topics will include how to grow suitable crystals, limits of detection, symmetry and space group concepts, parameters for determining structure quality and use of the technology in structural analysis, Applications will include compound identification, regio- and stereochemistry, crystal phases, (e.g. salt vs. co-crystal),and solvates.

This course will benefit chemists, scientists, and managers who are involved in the elucidation of small molecule structures. The course is designed for beginners interested in a fundamental introduction to single crystal X-ray and current capabilities of the technology. Students will benefit by learning about state of the art capabilities and applications.

1. Introduction
     * Historical Perspective
2. Instrumentation
     * Diffactometers and peripherials
     * Choosing an X-ray source
     * Cryo-cooling
3. Growing Suitable Crystals
     * How to approach a problem
     * Solvent Selection
     * Amount of sample
4. Introduction to Fundamentals of Single Crystal X-Ray
     * Braggs Law
     * Bravais lattice
     * Point group symmetry
     * Space groups symmetry
5. Defining a Good Structure
     * R factors
     * Software
     * Goodness of fit
     * Flack factor
6. Applications/Examples
     * Stereochemistry/absolute configuration
     * Complimentary to other solid state technologies (e.g. PXRD, ssNMR, etc.) in defining solid phases, H-bonding, co-crystals, etc.
     * Complimentary to NMR in defining intra and inter-molecular interactions (solution vs. solid)
     * Molecular packing (ability to accommodate solvent)
     * Simulated PXRD (complimentary with experimental PXRD)

Dr. Nina C. Gonnella is a Senior Research Fellow at Boehringer Ingelheim. She heads the NMR group (consisting of solution, solid state and LC-NMR capability) as well as sharing co-responsibility for the Single Crystal X-ray facility.  Her prior experience includes Ciba-Geigy/Novartis where she managed an NMR group in areas that included: small molecule characterization, protein-ligand structure elucidation and in-vivo drug metabolism. Nina held a position as adjunct professor at the University of Medicine & Dentistry of NJ (UMDNJ) (Graduate Program) where she participated in a graduate lecture series on structure based drug design. She subsequently joined Abbott Laboratories (Worcester Massachusetts) as a Group Leader of an NMR-LCMS group with focus on elucidating chemical structures and conducting protein-ligand binding studies. She has served on scientific review boards including an NIH Grant Review Committee as a primary reviewer. She has authored and co-authored over 70 peer review journal articles, authored a book chapter, as well as a book entitled “LC-NMR: Expanding the Limits of Structure Elucidation” CRC press 2013.