4LUE
Crystal Structure of HCK in complex with 7-[trans-4-(4-methylpiperazin-1-yl)cyclohexyl]-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-amine (resulting from displacement of SKF86002)
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 | 2013-02-01 |
Detector | RAYONIX MX-225 |
Wavelength(s) | 1.0 |
Spacegroup name | P 21 21 21 |
Unit cell lengths | 73.400, 93.530, 181.490 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 46.765 - 3.040 |
R-factor | 0.208 |
Rwork | 0.205 |
R-free | 0.25620 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 3vs3 |
RMSD bond length | 0.003 |
RMSD bond angle | 0.646 |
Data reduction software | MOSFLM |
Data scaling software | SCALA (3.3.20) |
Phasing software | PHASER (2.5.2) |
Refinement software | PHENIX (1.8.2_1309) |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 90.745 | 57.068 | 3.200 |
High resolution limit [Å] | 3.040 | 9.610 | 3.040 |
Rmerge | 0.034 | 0.374 | |
Rmeas | 0.037 | 0.405 | |
Rpim | 0.014 | 0.153 | |
Total number of observations | 5729 | 24488 | |
Number of reflections | 24812 | ||
<I/σ(I)> | 12.5 | 22.3 | 5 |
Completeness [%] | 100.0 | 99.5 | 100 |
Redundancy | 7 | 6.4 | 6.9 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, SITTING DROP | 8 | 288 | 0.1M Tris, 0.1M Calcium Acetate, 20% Glycerol, 24% PEG 6000, 2mM SKF86002, soaked with 2mM inhibitor in DMSO., pH 8.0, VAPOR DIFFUSION, SITTING DROP, temperature 288K |