4WIV
Crystal Structure of the first bromodomain of human BRD4 in complex with a novel inhibitor UMB32 (N-TERT-BUTYL-2-[4-(3,5-DIMETHYL-1,2-OXAZOL-4-YL) PHENYL]IMIDAZO[1,2-A]PYRAZIN-3-AMINE)
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | APS BEAMLINE 24-ID-E |
Synchrotron site | APS |
Beamline | 24-ID-E |
Temperature [K] | 100 |
Detector technology | CCD |
Collection date | 2014-02-14 |
Detector | ADSC QUANTUM 315 |
Wavelength(s) | 0.9792 |
Spacegroup name | P 21 21 21 |
Unit cell lengths | 43.562, 49.210, 60.991 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 35.449 - 1.560 |
R-factor | 0.1714 |
Rwork | 0.170 |
R-free | 0.20130 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 3mxf |
RMSD bond length | 0.007 |
RMSD bond angle | 1.296 |
Refinement software | PHENIX ((phenix.refine: 1.9_1678)) |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 35.450 | 1.616 |
High resolution limit [Å] | 1.560 | 1.560 |
Number of reflections | 19177 | |
<I/σ(I)> | 9.88 | 1.62 |
Completeness [%] | 99.6 | 100 |
Redundancy | 3.9 | 3.9 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, SITTING DROP | 7.4 | 295 | Crystals of inhibitor-free BRD4-BD1 were first obtained in a drop with equal volumes of BD1 at 12 mg/ml and a precipitant solution containing 100mM sodium nitrate, 5% ethylene glycol, and 18% (w/v) PEG3350, as precipitant. Rod-like crystals were typically grown in 10 days reaching a maximal size of 0.05x0.05x0.4 mm3. Then, native crystals were transferred and soaked in 1 mM UMB32 in the same crystallization buffer for 7 days. |