6X3P
Co-structure of BTK kinase domain with L-005298385 inhibitor
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | APS BEAMLINE 17-ID |
| Synchrotron site | APS |
| Beamline | 17-ID |
| Temperature [K] | 100 |
| Detector technology | PIXEL |
| Collection date | 2013-06-14 |
| Detector | DECTRIS PILATUS 6M |
| Wavelength(s) | 1. |
| Spacegroup name | P 21 21 2 |
| Unit cell lengths | 72.010, 104.640, 38.000 |
| Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
| Resolution | 42.330 - 1.340 |
| R-factor | 0.2048 |
| Rwork | 0.204 |
| R-free | 0.21740 |
| Structure solution method | FOURIER SYNTHESIS |
| RMSD bond length | 0.010 |
| RMSD bond angle | 1.100 |
| Data reduction software | XDS |
| Data scaling software | Aimless (0.1.27) |
| Phasing software | BUSTER-TNT |
| Refinement software | BUSTER |
Data quality characteristics
| Overall | Inner shell | Outer shell | |
| Low resolution limit [Å] | 42.330 | 42.330 | 1.430 |
| High resolution limit [Å] | 1.340 | 3.790 | 1.340 |
| Rmerge | 0.094 | 0.066 | 0.469 |
| Rmeas | 0.105 | 0.073 | 0.558 |
| Rpim | 0.047 | 0.030 | 0.296 |
| Total number of observations | 287858 | 18086 | 38736 |
| Number of reflections | 64654 | 3123 | 11536 |
| <I/σ(I)> | 9.3 | 22.9 | 2.3 |
| Completeness [%] | 99.0 | 99.5 | 99 |
| Redundancy | 4.5 | 5.8 | 3.4 |
| CC(1/2) | 0.994 | 0.995 | 0.758 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, HANGING DROP | 6.5 | 277 | 0.1 M Bis-Tris.Cl at pH 6.5, 2 mM TCEP Cl, 6% w/v PEG 20K, 10mM (S)-4-(8-amino-3-(1-(4-(dimethylamino)butanoyl)pyrrolidin-2-yl)imidazo[1,5-a]pyrazin-1-yl)-N-(thiazol-2-yl)benzamide, 5%v/v deuterated-DMSO,protein:precipitant volume ratio=1:2 |
