5DLX
FIRST DOMAIN OF HUMAN BROMODOMAIN BRD4 IN COMPLEX WITH INHIBITOR N-{3-[4-(3-chlorophenyl)piperazin-1-yl]propyl}-1-{3-methyl-[1,2,4]triazolo[4,3-b]pyridazin-6-yl}piperidine-4-carboxamide
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | ESRF BEAMLINE ID23-2 |
Synchrotron site | ESRF |
Beamline | ID23-2 |
Temperature [K] | 100 |
Detector technology | PIXEL |
Collection date | 2015-04-15 |
Detector | DECTRIS PILATUS 2M |
Wavelength(s) | 0.967700 |
Spacegroup name | P 21 21 21 |
Unit cell lengths | 41.723, 48.509, 58.094 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 37.230 - 1.900 |
R-factor | 0.12959 |
Rwork | 0.125 |
R-free | 0.20707 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 2oss |
RMSD bond length | 0.028 |
RMSD bond angle | 2.316 |
Data reduction software | XDS (jun 17, 2015) |
Data scaling software | XDS (jun 17, 2015) |
Phasing software | PHASER (version 2.5.6) |
Refinement software | REFMAC (5.8.0131) |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 50.000 | 2.020 |
High resolution limit [Å] | 1.900 | 1.900 |
Number of reflections | 9664 | |
<I/σ(I)> | 20.09 | 3.73 |
Completeness [%] | 99.3 | 97.8 |
Redundancy | 4.83 | 4.59 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 7.5 | 292 | Ratio 1:1 (protein:precipitant). 12 mg/mL Brd4_BD1 protein. Protein buffer 10 mM HEPES (pH 7.5) 150 mM NaCl. Precipitant agent 22 % (w/v) PEG 3350, 10% (w/v) ethylene glycol 30 % (w/v), 0.3 M NaFormate. 1.0 mM inhibitor (in DMSO) final concentration. Cryoprotection with 10 % (w/v) glycerol |