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Individual atomic positions for ligand have been lost
Lost of chemically useful information
Limiting the Resolution of the Data
Limited qmax = 9.59° Resolution = 3.0 Å Only metal position is
Effect of Limiting Resolution of the Data
Electron Density Map using all available data (qmax = 32.35°)
Resolution = 0.66 Å
All atomic positions are easily resolved
positions are still resolvable
Limiting the Resolution of the Data
Limited qmax = 14.48° Resolution = 2.0 Å
Metal position resolvable
Only gross shape of organic ligand evident
minimum resolution
Limiting the Resolution of the Data
Limited qmax = 19.47° Resolution = 1.5 Å Peaks start to “melt”
into each other Individual atomic
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
Discerning individual atomic position requires data resolution which is greater than the bond lengths between the atoms (.e.g C-C = 1.54Å)
The Effect of Limiting the Resolution of the Data
discernible Ligand is completely
“washed out”
Limiting the Resolution of the Data
Limited qmax = 8.21° Resolution = 3.5 Å Metal electron density
is “bleeding” into the traces of the ligand's electron density
Very often, but not always shows regular faces and edges
Why do youБайду номын сангаасneed good crystals anyway?
Quality of sample characterized by maximum diffraction angle (q) -- also expressed in “resolution” (Å)
Limiting the Resolution of the Data
Limited qmax = 25.0° Resolution = 0.84 Å Peaks are beginning
to flatten out Atomic positions are
still easily resolvable IUCr recommended
The larger the max. diffraction angle, the greater the resolution and the greater number of data (which is necessary to adequately model the structure)
Limiting the Resolution of the Data
Limited qmax = 7.18° Resolution = 4.0 Å Metal position is only
barely above background No trace of ligand
Limiting the Resolution of the Data
Peak positions for ligand have shifted away from true atomic positions
Limiting the Resolution of the Data
Limited qmax = 11.54° Resolution = 2.5 Å
Metal position still discernible
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
Lost of chemically useful information
Limiting the Resolution of the Data
Limited qmax = 9.59° Resolution = 3.0 Å Only metal position is
Effect of Limiting Resolution of the Data
Electron Density Map using all available data (qmax = 32.35°)
Resolution = 0.66 Å
All atomic positions are easily resolved
positions are still resolvable
Limiting the Resolution of the Data
Limited qmax = 14.48° Resolution = 2.0 Å
Metal position resolvable
Only gross shape of organic ligand evident
minimum resolution
Limiting the Resolution of the Data
Limited qmax = 19.47° Resolution = 1.5 Å Peaks start to “melt”
into each other Individual atomic
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
Discerning individual atomic position requires data resolution which is greater than the bond lengths between the atoms (.e.g C-C = 1.54Å)
The Effect of Limiting the Resolution of the Data
discernible Ligand is completely
“washed out”
Limiting the Resolution of the Data
Limited qmax = 8.21° Resolution = 3.5 Å Metal electron density
is “bleeding” into the traces of the ligand's electron density
Very often, but not always shows regular faces and edges
Why do youБайду номын сангаасneed good crystals anyway?
Quality of sample characterized by maximum diffraction angle (q) -- also expressed in “resolution” (Å)
Limiting the Resolution of the Data
Limited qmax = 25.0° Resolution = 0.84 Å Peaks are beginning
to flatten out Atomic positions are
still easily resolvable IUCr recommended
The larger the max. diffraction angle, the greater the resolution and the greater number of data (which is necessary to adequately model the structure)
Limiting the Resolution of the Data
Limited qmax = 7.18° Resolution = 4.0 Å Metal position is only
barely above background No trace of ligand
Limiting the Resolution of the Data
Peak positions for ligand have shifted away from true atomic positions
Limiting the Resolution of the Data
Limited qmax = 11.54° Resolution = 2.5 Å
Metal position still discernible
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