Macromolecular Crystallization and Crystal Perfection
, by Chayen, Naomi E; Helliwell, John R; Snell, Edward H- ISBN: 9780199213252 | 0199213259
- Cover: Hardcover
- Copyright: 5/20/2010
Naomi E. Chayen is Professor of Biomedical Sciences at Imperial College London, Visiting Professor at Harvard Medical School and the President of the International Organisation for Biological Crystallization (IOBCr). She organises and chairs crystallization sessions at international conferences and courses, and is a Crystallization Co-Editor of Acta Crystallographica D.
Professor J.R. Helliwell is Professor of Structural Chemistry at the University of Manchester and an Honorary Visiting Scientist at the STFC Daresbury Laboratory. He has served as Editor-in-Chief of Acta Crystallographica and is currently President of the European Crystallographic Association.
Dr. Edward Snell is Assistant Professor at the Hauptman-Woodward Medical Research Institute at the State University of New York at Buffalo. He has worked at NASA as a senior scientist and was PI on several space missions on the International Space station. He has received a number of academic awards.
Preface | p. ix |
Acknowledgements | p. xi |
Introduction and Overview | |
Introduction | p. 3 |
Crystal growth | p. 4 |
Diffraction techniques | p. 6 |
X-rays | p. 6 |
Neutrons | p. 7 |
Crystal volume and quality | p. 9 |
Short-range order (intermolecular) | p. 10 |
Long-range order (domain structure) | p. 14 |
The combination of short- and long-range order | p. 16 |
Chapter summary | p. 17 |
Crystallization | |
Crystallization theory | p. 21 |
Chapter summary | p. 23 |
Practical methods of crystallization | p. 24 |
Batch | p. 24 |
Vapour diffusion | p. 25 |
Dialysis | p. 26 |
Free interface diffusion | p. 26 |
Converting between methods | p. 27 |
Chapter summary | p. 28 |
Screening | p. 29 |
Screens: problems and new developments | p. 29 |
Automation-and miniaturization of screening procedures | p. 29 |
The effect of high-throughput: crystallization robotics | p. 34 |
Analysis of large quantities of crystallization data | p. 34 |
Experiment volume considerations | p. 37 |
Imaging and monitoring of crystallization trials | p. 37 |
Chapter summary | p. 37 |
Optimization | p. 38 |
Practical uses of the crystallization phase diagram | p. 38 |
Methods for separating nucleation and growth | p. 40 |
Seeding | p. 41 |
Dilution techniques | p. 42 |
The application o flight-scattering techniques | p. 44 |
Static light scattering | p. 44 |
Dynamic light scattering | p. 44 |
Chapter summary | p. 47 |
Strategies to apply when high-quality crystals cannot be obtained | p. 48 |
Introduction | p. 48 |
Non-covalent modification of the sample | p. 48 |
Covalent modification of the sample | p. 49 |
Reductive methylation | p. 49 |
General chemical modification | p. 50 |
Mutagenesis, domain refinement and homologues | p. 50 |
Surface-entropy reduction | p. 50 |
Proteolysis | p. 51 |
Orthologues and homologues | p. 51 |
Antibody fragments | p. 52 |
Chapter summary | p. 52 |
Membrane proteins | p. 53 |
Introduction | p. 53 |
Crystallization | p. 53 |
Screening with detergents | p. 55 |
Lipidic cubic-phase crystallization | p. 55 |
Antibody fragment approaches | p. 56 |
Characterization using neutron-enhanced contrast | p. 56 |
Chapter summary | p. 56 |
Alternative approaches | p. 58 |
Gel growth | p. 58 |
Microgravity | p. 59 |
Interferometry | p. 59 |
Depletion zone | p. 60 |
Microfluidics | p. 61 |
Magnetic and electric fields | p. 62 |
Chapter summary | p. 64 |
Diffraction | |
Experimental aspects | p. 67 |
The diffraction pattern | p. 67 |
Structural detail | p. 70 |
Determining structure when the resolution is not ideal | p. 72 |
How accurate is the structure? | p. 73 |
Chapter summary | p. 76 |
Analysis of the molecular short-range order | p. 78 |
Structural data | p. 78 |
Thermal motion and diffuse scattering | p. 79 |
Diffuse scattering as a source of measurement error in the Bragg intensities | p. 81 |
Chapter summary | p. 82 |
Analysis of long-range order | p. 83 |
Reflection profiling | p. 83 |
Topography | p. 88 |
Photography-based topography | p. 89 |
Digital-based topography | p. 90 |
Reciprocal-space mapping | p. 91 |
Combinational analysis and chapter summary | p. 94 |
Macromolecular crystals and twinning | p. 96 |
Historical examples | p. 97 |
Types of twinning | p. 98 |
The twin fraction and testing for twinned data | p. 102 |
Using twinned data | p. 104 |
Overcoming twinning in crystals | p. 105 |
How prevalent is twinning? | p. 109 |
Chapter summary | p. 110 |
Other macromolecular crystal diffraction disorders | p. 112 |
Introduction | p. 112 |
Case studies | p. 112 |
Chapter summary | p. 118 |
Degradation and improvement of crystal perfection | p. 119 |
Ageing | p. 119 |
Radiation damage | p. 119 |
Cryo-cooling | p. 124 |
Dehydration and humidity control | p. 127 |
Chapter summary | p. 131 |
Unusual diffraction geometries | p. 132 |
Chapter summary | p. 136 |
Making the most of difficult crystals - beamline and detector optimization | p. 137 |
Introduction | p. 137 |
Geometry and end-station instrumentation | p. 137 |
Signal and noise considerations | p. 138 |
Very small crystal volume'microcrystals' | p. 143 |
Phasing and the available instrumentation | p. 147 |
Robotics, telepresence and remote access | p. 148 |
More specialized applications | p. 149 |
Chapter summary | p. 150 |
Protein powders-making the most of tiny crystallites in bulk | p. 151 |
Introduction | p. 151 |
Quantitative protein powder analyses have opened up in recent years | p. 152 |
Structure determination of unknown proteins? | p. 154 |
Characterization of protein crystal polymorphism | p. 155 |
Chapter summary | p. 156 |
Complementary techniques | p. 158 |
Chapter summary | p. 159 |
The Future | |
The X-ray laser and the single molecule - no crystal needed? | p. 163 |
Overall summary and future thoughts | p. 168 |
Glossary of abbreviations, terms and symbols | p. 170 |
Abbreviations | p. 170 |
General | p. 170 |
Synchrotron sources | p. 171 |
Neutron sources | p. 171 |
Terms | p. 171 |
Crystallization | p. 171 |
X-ray analysis | p. 172 |
Symbols | p. 173 |
Crystallization and crystal-growth-monitoring symbols | p. 173 |
Diffraction symbols | p. 174 |
References | p. 175 |
Index | p. 219 |
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