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 |
