3PJ1
Crystal structure of BTK kinase domain complexed with 3-(2,6-Dichloro-phenyl)-7-[4-(2-diethylamino-ethoxy)-phenylamino]-1-methyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-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) | 0.9804 |
| Spacegroup name | P 21 21 2 |
| Unit cell lengths | 71.728, 104.818, 38.170 |
| Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
| Resolution | 40.000 - 2.000 |
| R-factor | 0.22323 |
| Rwork | 0.221 |
| R-free | 0.25685 |
| Structure solution method | FOURIER SYNTHESIS |
| Starting model (for MR) | 3pix |
| RMSD bond length | 0.007 |
| RMSD bond angle | 0.976 |
| 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 | 2.070 |
| High resolution limit [Å] | 2.000 | 2.000 |
| Number of reflections | 20034 | |
| <I/σ(I)> | 13.2 | 2.8 |
| Completeness [%] | 99.6 | 96.8 |
| Redundancy | 6.9 | 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 |
