晶体生长过程视频.ppt

Growing X-ray Quality Crystals Paul D. Boyle Department of Chemistry North Carolina State University 15 November 2006 Topics to be Covered The Objective: Getting “Good” Crystals Why do you need good crystals anyway? The Right Attitude toward crystal growing Factors affecting crystallization Crystal growing techniques Questions and Answers/Discussion Objective: Getting Good Crystals A “good” crystal is: 0.1-0.4 mm in at least 2 of its dimensions exhibits a high degree of internal order as evidenced by the presence of an X-ray diffraction pattern Very often, but not always shows regular faces and edges Why do you need good crystals anyway? Quality of sample characterized by maximum diffraction angle (q) -- also expressed in “resolution” (?) The larger the max. diffraction angle, the greater the resolution and the greater number of data (which is necessary to adequately model the structure) Discerning individual atomic position requires data resolution which is greater than the bond lengths between the atoms (.e.g C-C = 1.54?) The Effect of Limiting the Resolution of the Data Effect of Limiting Resolution of the Data Electron Density Map using all available data (qmax = 32.35°) Resolution = 0.66 ? All atomic positions are easily resolved Limiting the Resolution of the Data Limited qmax = 25.0° Resolution = 0.84 ? Peaks are beginning to flatten out Atomic positions are still easily resolvable IUCr recommended minimum resolution Limiting the Resolution of the Data Limited qmax = 19.47° Resolution = 1.5 ? Peaks start to “melt” into each other Individual atomic positions are still resolvable Limiting the Resolution of the Data Limited qmax = 14.48° Resolution = 2.0 ? Metal position resolvable Only gross shape of organic ligand evident Peak positions for ligand have shifted away from true atomic positions Limiting the Resolution of the Data Limited qmax = 11.54° Resolution = 2.5 ? Metal position still discernible Individual atomic positions for ligand have been lost Lost o