Chemistry 6181MWF 9:05 Spring 2003
General Information
Instructor:Angus Wilkinson, Rm 2-61 Boggs; Phone: 894-4036;
E-mail:
Classroom:3-46
Texts:Primarily "Crystal Structure Analysis for Chemists and Biologists", by Glusker, Lewis and Rossi, VCH. "International Tables for Crystallography, Vol. A, Teaching Edition" will also be used.
Grading:Homework:(10%) Problem assignments will be given in class one week before the work is due.
Projects: 10% for completion of silver carboxylate / lead thiolate Project: 10% for single crystal structure determination.
"Hour Exams": (total 40%) Two exams will be given during normal class periods.
Final Exam: (30%) The exam will be given during the scheduled exam period: Friday, May 1st, 2:50 - 5:40.
Review sessions:Review session will be held if requested. Students will be expected to specify exactly what they want reviewing.
Help:The instructor will be available to answer questions by appointment.
Lecture topics to be covered
Introduction to crystal structure analysis - Chapter 1
Crystals - Chapter 2
Diffraction by Crystals - Chapter 3
Symmetry in Crystals and their Diffraction Patterns - Chapter 4 and Int. Tab. Vol A
Combining Waves to make an Image - Chapter 6
Measurement of Structure Amplitudes - Chapter 7
Estimation of Relative Phase Angles - Chapter 8
Electron-Density Maps - Chapter 9
Least Squares Refinement of Structures - Chapter 10
Interpreting x, y and z - Chapter 11
Temperature factors - Chapter 13
Chirality and Absolute Structure - Chapter 14
The Rietveld method - from handouts
Synchrotron X-rays and neutrons - from handouts
Resonant scattering for MAD phasing and cation substitution problems - from handouts
Projects
1) Collection of data and solution of a structure using EXCEL. This will provide an Introduction to the Inner workings of modern black box computer programs.
Prepare sample of silver behnate or a lead thiolate.
Collect powder pattern
Fit peaks to get positions and Intensities
Index peaks to determine a unit cell
Calculate structure factors from Integrated Intensities
Calculate 1D Patterson map to find heavy atoms
Perform Fourier synthesis to locate other atoms
Calculate an R-factor for your model
2) Solve a single crystal structure.
Collect single crystal X-ray diffraction data for a simple organic compound. Solve structure using modern "black box" programs.
Refine structure
Prepare tables and figures for publications
Project one should be started at the beginning of the semester and worked on as you become familiar with the theory.
Project two should be started towards the end of the theory lectures.
Resource books for crystallography
Course texts
1) "Crystal Structure Analysis for Chemists and Biologists", Glusker, Lewis and Rossi, VCH, 1994.
2) "International Tables for Crystallography", brief teaching edition, Vol. A, Kluwer, 1993.
- the full version just has additional space groups. The notes are the same.
Other books
3) "Crystal Structure Analysis A Primer", Glusker and Truebllod, Oxford,, 1985.
This book is a simpler version of book 1).
4) "X-ray Structure Determination A Practical Guide", Stout and Jensen, Wiley, 1989.
A good introductory book.
5) "Fundamentals of Crystallography", ed. Giacovazzo, Oxford Scientific Publications, 1992.
A good crystallography book, but not for absolute beginers
6) "Structure Determination by X-ray Crystallography", Ladd and Palmer, Plenum, 1994.
A reasonable book. Aimed at possible practioners not people who just need an overview.
7) "X-ray Diffraction", Warren, Dover, 1990.
A classic. Very mathematical. It is about X-ray scattering not crystal structure determination.
8) "Elements of X-ray Diffraction", Cullity and Stock, Prentice-Hall, 2001.
-Primarily about powder diffraction
9) "The Rietveld Method", Ed. R. A. Young, Oxford Science Publications, 1993.
Devoted to Rietveld analysis. Rietveld analysis is an approach to extracting structural information from powder diffraction patterns. It requires that you already have a good knowledge of what the structure is like.
10) "Structure Determination from Powder Diffraction Data", Eds. David, Shankland, McCusker and Baerlocher, Oxford Science Publications, 2002.