3PJ2
Crystal structure of BTK kinase domain complexed with 2-[4-(2-Diethylamino-ethoxy)-phenylamino]-6-(4-fluoro-phenoxy)-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one
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 | 71.356, 104.803, 38.002 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 42.220 - 1.750 |
R-factor | 0.23086 |
Rwork | 0.229 |
R-free | 0.26307 |
Structure solution method | FOURIER SYNTHESIS |
Starting model (for MR) | 3pix |
RMSD bond length | 0.006 |
RMSD bond angle | 0.959 |
Data reduction software | DENZO |
Data scaling software | SCALEPACK |
Phasing software | REFMAC |
Refinement software | REFMAC |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 50.000 | 1.810 |
High resolution limit [Å] | 1.750 | 1.750 |
Number of reflections | 27449 | |
<I/σ(I)> | 15.6 | 2.4 |
Completeness [%] | 92.7 | 60 |
Redundancy | 3.9 | 2.2 |
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 |