6X3O
Co-structure of BTK kinase domain with L-005191930 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 | 2014-06-01 |
| Detector | DECTRIS PILATUS 6M |
| Wavelength(s) | 1. |
| Spacegroup name | P 1 21 1 |
| Unit cell lengths | 38.300, 72.010, 104.390 |
| Unit cell angles | 90.00, 91.40, 90.00 |
Refinement procedure
| Resolution | 34.790 - 1.900 |
| R-factor | 0.181 |
| Rwork | 0.179 |
| R-free | 0.21280 |
| Structure solution method | FOURIER SYNTHESIS |
| RMSD bond length | 0.010 |
| RMSD bond angle | 0.990 |
| 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] | 34.790 | 34.790 | 2.120 |
| High resolution limit [Å] | 1.900 | 4.250 | 1.900 |
| Rmerge | 0.069 | 0.035 | 0.320 |
| Rmeas | 0.084 | 0.043 | 0.391 |
| Rpim | 0.048 | 0.025 | 0.221 |
| Total number of observations | 130298 | 11360 | 36585 |
| Number of reflections | 44327 | 3982 | 12580 |
| <I/σ(I)> | 10.8 | 25.1 | 3.4 |
| Completeness [%] | 99.1 | 97.5 | 99.3 |
| Redundancy | 2.9 | 2.9 | 2.9 |
| CC(1/2) | 0.996 | 0.996 | 0.866 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, HANGING DROP | 7.5 | 277 | 0.1M BIS-TRIS CL pH 7.5, 18%w/vPEG 20,000, 5mM 4-(8-amino-3-((6R,8aS)-3-oxooctahydroindolizin-6-yl)imidazo[1,5-a]pyrazin-1-yl)-3-methoxy-N-(4-(trifluoromethyl)pyridin-2-yl)benzamide, 5mM (S)-4-(8-amino-3-(1-(4-(dimethylamino)butanoyl)pyrrolidin-2-yl)imidazo[1,5-a]pyrazin-1-yl)-N-(thiazol-2-yl)benzamide, 10% v/v deuterated-DMSO |
