5H09
Crystal structure of HCK complexed with a pyrrolo-pyrimidine inhibitor (S)-ethyl2-(((1r,4S)-4-(4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl)cyclohexyl)amino)-4-methylpentanoate
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | PHOTON FACTORY BEAMLINE AR-NE3A |
| Synchrotron site | Photon Factory |
| Beamline | AR-NE3A |
| Temperature [K] | 100 |
| Detector technology | CCD |
| Collection date | 2014-02-16 |
| Detector | ADSC QUANTUM 270 |
| Wavelength(s) | 0.91 |
| Spacegroup name | P 21 21 21 |
| Unit cell lengths | 43.037, 85.425, 128.840 |
| Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
| Resolution | 28.640 - 1.945 |
| R-factor | 0.1917 |
| Rwork | 0.190 |
| R-free | 0.22270 |
| Structure solution method | MOLECULAR REPLACEMENT |
| Starting model (for MR) | 3vs3 |
| RMSD bond length | 0.003 |
| RMSD bond angle | 0.631 |
| Data reduction software | HKL-2000 |
| Data scaling software | HKL-2000 |
| Phasing software | PHASER (2.5.5) |
| Refinement software | PHENIX (1.11.1_2575) |
Data quality characteristics
| Overall | Inner shell | Outer shell | |
| Low resolution limit [Å] | 50.000 | 50.000 | 1.980 |
| High resolution limit [Å] | 1.950 | 5.290 | 1.950 |
| Rmerge | 0.116 | 0.070 | 0.914 |
| Rmeas | 0.126 | 0.077 | 0.986 |
| Rpim | 0.047 | 0.031 | 0.367 |
| Total number of observations | 254528 | ||
| Number of reflections | 35580 | 1921 | 1747 |
| <I/σ(I)> | 7.4 | ||
| Completeness [%] | 99.9 | 97.6 | 100 |
| Redundancy | 7.2 | 6.1 | 7.2 |
| CC(1/2) | 0.995 | 0.777 |
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 |
