X-Ray Crystallography

3.

The Crystallographic Experiment

3.1.

Crystal Growth and Preparation

3.1.1.

Importance of High-Quality Crystals

3.1.1.1.

Criteria for Crystal Quality

3.1.1.2.

Effects of Defects and Imperfections

3.1.2.

Common Crystallization Methods

3.1.2.1.

Vapor Diffusion

3.1.2.1.1.

Hanging Drop Method

3.1.2.1.2.

Sitting Drop Method

3.1.2.2.

Microbatch Method

3.1.2.3.

Dialysis Method

3.1.2.4.

Batch Crystallization

3.1.2.5.

Seeding Techniques

3.1.3.

Crystal Handling and Mounting

3.1.3.1.

Tools and Techniques

3.1.3.2.

Minimizing Mechanical Damage

3.1.3.3.

Mounting Loops and Capillaries

3.1.4.

Cryo-protection

3.1.4.1.

Purpose and Principles

3.1.4.2.

Common Cryo-protectants

3.1.4.3.

Flash Cooling Techniques

3.2.

X-Ray Sources and Instrumentation

3.2.1.

Laboratory Sources

3.2.1.1.

Sealed X-ray Tubes

3.2.1.1.1.

Operation and Maintenance

3.2.1.1.2.

3.2.1.2.

Rotating Anode Generators

3.2.1.2.1.

Increased Intensity

3.2.1.2.2.

Cooling Requirements

3.2.2.

Synchrotron Radiation

3.2.2.1.

Properties and Advantages

3.2.2.1.1.

High Intensity and Tunability

3.2.2.1.2.

Time-Resolved Experiments

3.2.2.2.

Beamline Components

3.2.2.2.1.

3.2.2.2.2.

Mirrors and Focusing Optics

3.2.2.2.3.

Sample Environment

3.2.3.

The Diffractometer

3.2.3.1.

3.2.3.1.1.

3.2.3.1.2.

Sample Orientation

3.2.3.2.

3.2.3.2.1.

3.2.3.2.2.

3.2.3.2.3.

Focusing Devices

3.2.3.3.

3.2.3.3.1.

3.2.3.3.2.

3.2.3.3.3.

3.2.3.3.4.

Pixel Array Detectors

3.2.3.3.5.

Detector Calibration and Performance

3.3.

Data Collection

3.3.1.

Crystal Screening and Characterization

3.3.1.1.

Assessing Crystal Quality

3.3.1.2.

Unit Cell Determination

3.3.1.3.

Mosaicity Measurement

3.3.2.

Data Collection Strategy

3.3.2.1.

Oscillation Range

3.3.2.1.1.

Rotation Methods

3.3.2.1.2.

Coverage of Reciprocal Space

3.3.2.2.

3.3.2.2.1.

Signal-to-Noise Considerations

3.3.2.2.2.

Radiation Sensitivity

3.3.2.3.

Detector Distance

3.3.2.3.1.

Resolution Considerations

3.3.2.3.2.

Spot Separation

3.3.2.4.

Redundancy and Completeness

3.3.3.

Monitoring Radiation Damage

3.3.3.1.

Signs of Damage

3.3.3.2.

Strategies to Minimize Damage

3.3.4.

Data Completeness and Redundancy

3.3.4.1.

Importance for Structure Solution

3.3.4.2.

Strategies to Maximize Data Quality

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4. Data Processing and Structure Solution