3PIX
Crystal structure of BTK kinase domain complexed with 2-Isopropyl-7-(4-methyl-piperazin-1-yl)-4-(5-methyl-2H-pyrazol-3-ylamino)-2H-phthalazin-1-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 | 70.028, 104.430, 37.953 |
| Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
| Resolution | 37.960 - 1.850 |
| Rwork | 0.227 |
| R-free | 0.26561 |
| Structure solution method | MOLECULAR REPLACEMENT |
| Starting model (for MR) | 1k2p |
| RMSD bond length | 0.007 |
| RMSD bond angle | 1.086 |
| Data reduction software | DENZO |
| Data scaling software | SCALEPACK |
| Phasing software | PHASER |
| Refinement software | REFMAC (5.2.0019) |
Data quality characteristics
| Overall | Outer shell | |
| Low resolution limit [Å] | 40.000 | 1.920 |
| High resolution limit [Å] | 1.850 | 1.850 |
| Number of reflections | 22572 | |
| <I/σ(I)> | 13.7 | 2.1 |
| Completeness [%] | 92.6 | 63.2 |
| Redundancy | 5.2 | 3.6 |
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 |
