7N5Y
Fragment-Based Drug Design of a Novel, Covalent Bruton's Tyrosine Kinase Inhibitor
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | ALS BEAMLINE 5.0.3 |
Synchrotron site | ALS |
Beamline | 5.0.3 |
Temperature [K] | 100 |
Detector technology | CCD |
Collection date | 2012-12-01 |
Detector | ADSC QUANTUM 315r |
Wavelength(s) | 0.976 |
Spacegroup name | P 21 21 2 |
Unit cell lengths | 72.717, 104.729, 38.050 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 30.000 - 1.850 |
R-factor | 0.1646 |
Rwork | 0.163 |
R-free | 0.20150 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 4z3v |
RMSD bond length | 0.007 |
RMSD bond angle | 1.426 |
Data reduction software | HKL-2000 |
Data scaling software | HKL-2000 |
Phasing software | MOLREP |
Refinement software | REFMAC (5.8.0267) |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 50.000 | 50.000 | 1.850 |
High resolution limit [Å] | 1.820 | 4.940 | 1.820 |
Rmerge | 0.123 | 0.045 | 0.650 |
Total number of observations | 151880 | ||
Number of reflections | 26776 | 1483 | 1275 |
<I/σ(I)> | 7.4 | ||
Completeness [%] | 99.9 | 99.2 | 99 |
Redundancy | 5.7 | 5.5 | 3.6 |
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 and 0.12M alcohol mixture |