3EMG
Discovery and SAR of novel 4-thiazolyl-2-phenylaminopyrimidines as potent inhibitors of spleen tyrosine kinase (SYK)
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | ALS BEAMLINE 5.0.2 |
Synchrotron site | ALS |
Beamline | 5.0.2 |
Temperature [K] | 200 |
Detector technology | CCD |
Collection date | 2003-12-15 |
Detector | ADSC QUANTUM 315 |
Wavelength(s) | 1.0000 |
Spacegroup name | P 1 21 1 |
Unit cell lengths | 39.870, 84.450, 41.440 |
Unit cell angles | 90.00, 99.63, 90.00 |
Refinement procedure
Resolution | 39.305 - 2.600 |
R-factor | 0.1996 |
Rwork | 0.200 |
R-free | 0.22170 |
Structure solution method | FOURIER SYNTHESIS |
Starting model (for MR) | in-house apo structure of SYK |
Data reduction software | MOSFLM |
Data scaling software | SCALA |
Phasing software | CNS |
Refinement software | CNS |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 39.305 | 2.740 |
High resolution limit [Å] | 2.600 | 2.600 |
Rmerge | 0.058 | 0.135 |
Total number of observations | 4079 | |
Number of reflections | 15406 | |
<I/σ(I)> | 4.525 | 2.3 |
Completeness [%] | 94.0 | 92.9 |
Redundancy | 1.9 | 1.8 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 7 | 298 | 10 mg/mL Protein, 15-20% PEG 8000, 100 mM Sodium nitrate, 100 mM HEPES pH 7.0, VAPOR DIFFUSION, HANGING DROP, temperature 298.0K |