4Z3V
Fragment-Based Discovery of a Small Molecule Reversible Inhibitor of Bruton's Tyrosine Kinase
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | APS BEAMLINE 23-ID-B |
| Synchrotron site | APS |
| Beamline | 23-ID-B |
| Temperature [K] | 100 |
| Detector technology | CCD |
| Collection date | 2012-02-08 |
| Detector | MARMOSAIC 300 mm CCD |
| Wavelength(s) | 1.033 |
| Spacegroup name | P 21 21 2 |
| Unit cell lengths | 73.092, 104.100, 38.078 |
| Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
| Resolution | 30.000 - 1.600 |
| R-factor | 0.1663 |
| Rwork | 0.165 |
| R-free | 0.19750 |
| Structure solution method | MOLECULAR REPLACEMENT |
| Starting model (for MR) | 3gen |
| RMSD bond length | 0.008 |
| RMSD bond angle | 1.286 |
| Data reduction software | HKL-2000 |
| Data scaling software | HKL-2000 |
| Phasing software | PHASER (2.3.0) |
| Refinement software | REFMAC (5.7.0025) |
Data quality characteristics
| Overall | |
| Low resolution limit [Å] | 50.000 |
| High resolution limit [Å] | 1.550 |
| Rmerge | 0.097 |
| Total number of observations | 267114 |
| Number of reflections | 40885 |
| <I/σ(I)> | 9.5 |
| Completeness [%] | 95.0 |
| Redundancy | 6.5 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, HANGING DROP | 6.5 | 277 | 10% polyethylene glycol 4000, 20% glycerol, 0.1M imidazole/MES, pH 6.5, 0.12M alcohol mixture |
