5H0H
Crystal structure of HCK complexed with a pyrrolo-pyrimidine inhibitor (S)-2-(((1r,4S)-4-(4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl)cyclohexyl)amino)-N,N,4-trimethylpentanamide
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | SPRING-8 BEAMLINE BL26B2 |
| Synchrotron site | SPring-8 |
| Beamline | BL26B2 |
| Temperature [K] | 100 |
| Detector technology | CCD |
| Collection date | 2015-01-23 |
| Detector | MARMOSAIC 225 mm CCD |
| Wavelength(s) | 1 |
| Spacegroup name | P 21 21 21 |
| Unit cell lengths | 43.113, 85.623, 129.010 |
| Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
| Resolution | 42.812 - 1.720 |
| R-factor | 0.1865 |
| Rwork | 0.185 |
| R-free | 0.22390 |
| Structure solution method | MOLECULAR REPLACEMENT |
| Starting model (for MR) | 3vs3 |
| RMSD bond length | 0.007 |
| RMSD bond angle | 0.996 |
| Data reduction software | HKL-2000 |
| Data scaling software | HKL-2000 |
| Phasing software | PHASER (2.5.6) |
| Refinement software | PHENIX (1.9_1690) |
Data quality characteristics
| Overall | Inner shell | Outer shell | |
| Low resolution limit [Å] | 50.000 | 50.000 | 1.750 |
| High resolution limit [Å] | 1.720 | 4.670 | 1.720 |
| Rmerge | 0.068 | 0.032 | 0.558 |
| Rmeas | 0.073 | 0.035 | 0.607 |
| Rpim | 0.027 | 0.013 | 0.234 |
| Total number of observations | 375872 | ||
| Number of reflections | 51602 | ||
| <I/σ(I)> | 9.3 | ||
| Completeness [%] | 99.9 | 99.6 | 99 |
| Redundancy | 7.3 | 6.8 | 6.5 |
| CC(1/2) | 0.999 | 0.861 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, SITTING DROP | 293 | 0.22-0.25 M ammonium formate, 12-22 % PEG 3350 |
