4RG0
Crystal structure of BTK kinase domain complexed with 2-[8-fluoro-2-[2-(hydroxymethyl)-3-[1-methyl-5-[[5-(4-methylpiperazin-1-yl)-2-pyridyl]amino]-6-oxo-3-pyridyl]phenyl]-1-oxo-3,4-dihydroisoquinolin-6-yl]-2-methyl-propanenitrile
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 | MARMOSAIC 325 mm CCD |
| Wavelength(s) | 0.97946 |
| Spacegroup name | P 21 21 2 |
| Unit cell lengths | 71.937, 106.339, 38.429 |
| Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
| Resolution | 42.760 - 2.500 |
| R-factor | 0.20306 |
| Rwork | 0.199 |
| R-free | 0.28223 |
| Structure solution method | FOURIER SYNTHESIS |
| Starting model (for MR) | 4otr |
| RMSD bond length | 0.011 |
| RMSD bond angle | 1.320 |
| Data reduction software | DENZO |
| Data scaling software | SCALEPACK |
| Phasing software | CNS |
| Refinement software | REFMAC (5.8.0048) |
Data quality characteristics
| Overall | Outer shell | |
| Low resolution limit [Å] | 42.760 | 2.565 |
| High resolution limit [Å] | 2.500 | 2.500 |
| Number of reflections | 9101 | |
| <I/σ(I)> | 5.6 | 1.6 |
| Completeness [%] | 88.8 | 63.66 |
| Redundancy | 3.4 | 2 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, HANGING DROP | 8 | 293 | 33% PEG3350, 0.1 M HEPES, pH 8.0, VAPOR DIFFUSION, HANGING DROP, temperature 293K |
