5VO2
DLK in complex with inhibitor 5-(1-isopropyl-5-(1-(oxetan-3-yl)piperidin-4-yl)-1H-pyrazol-3-yl)-3-(trifluoromethyl)pyridin-2-amine (compound 7)
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | SSRL BEAMLINE BL7-1 |
Synchrotron site | SSRL |
Beamline | BL7-1 |
Temperature [K] | 100 |
Detector technology | CCD |
Collection date | 2012-08-23 |
Detector | ADSC QUANTUM 315 |
Wavelength(s) | 1 |
Spacegroup name | P 1 21 1 |
Unit cell lengths | 57.290, 39.463, 60.113 |
Unit cell angles | 90.00, 104.81, 90.00 |
Refinement procedure
Resolution | 35.790 - 2.960 |
R-factor | 0.1743 |
Rwork | 0.170 |
R-free | 0.26370 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 5cen |
RMSD bond length | 0.009 |
RMSD bond angle | 1.020 |
Data reduction software | XDS |
Data scaling software | SCALA (3.3.20) |
Phasing software | PHASER |
Refinement software | BUSTER (2.11.5) |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 39.463 | 39.463 | 3.120 |
High resolution limit [Å] | 2.958 | 9.350 | 2.960 |
Rmerge | 0.019 | 0.312 | |
Rmeas | 0.135 | 0.027 | 0.409 |
Rpim | 0.071 | 0.015 | 0.212 |
Total number of observations | 19858 | ||
Number of reflections | 5586 | ||
<I/σ(I)> | 11.5 | 37.2 | 2.5 |
Completeness [%] | 99.5 | 98.1 | 100 |
Redundancy | 3.6 | 3.3 | 3.6 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, SITTING DROP | 7.7 | 293 | 20% PEG 3350, 0.2 M Mg Acetate, 0.1 M Hepes pH 7.7 |