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 |