3PIZ
Crystal structure of BTK kinase domain complexed with (5-Amino-1-o-tolyl-1H-pyrazol-4-yl)-[3-(1-methanesulfonyl-piperidin-4-yl)-phenyl]-methanone
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | SSRL BEAMLINE BL9-2 |
Synchrotron site | SSRL |
Beamline | BL9-2 |
Temperature [K] | 100 |
Detector technology | CCD |
Detector | ADSC QUANTUM 315 |
Wavelength(s) | 0.9795 |
Spacegroup name | P 21 21 2 |
Unit cell lengths | 71.267, 105.304, 38.054 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 38.040 - 2.210 |
R-factor | 0.22759 |
Rwork | 0.225 |
R-free | 0.28164 |
Structure solution method | FOURIER SYNTHESIS |
Starting model (for MR) | 3pix |
RMSD bond length | 0.008 |
RMSD bond angle | 1.010 |
Data reduction software | DENZO |
Data scaling software | SCALEPACK |
Phasing software | REFMAC |
Refinement software | REFMAC |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 40.000 | 2.280 |
High resolution limit [Å] | 2.200 | 2.200 |
Number of reflections | 13820 | |
<I/σ(I)> | 9 | 2.3 |
Completeness [%] | 91.6 | 61.8 |
Redundancy | 4 | 2.1 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 8 | 293 | 33% PEG3350, 0.1M HEPES, pH 8.0, VAPOR DIFFUSION, HANGING DROP, temperature 293K |