4X2I
Discovery of benzotriazolo diazepines as orally-active inhibitors of BET bromodomains: Crystal structure of BRD4 with CPI-13
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | APS BEAMLINE 22-ID |
| Synchrotron site | APS |
| Beamline | 22-ID |
| Temperature [K] | 100 |
| Detector technology | CCD |
| Collection date | 2012-01-23 |
| Detector | MARMOSAIC 300 mm CCD |
| Wavelength(s) | 1.00 |
| Spacegroup name | P 21 21 21 |
| Unit cell lengths | 33.905, 48.181, 78.314 |
| Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
| Resolution | 41.040 - 1.200 |
| R-factor | 0.14065 |
| Rwork | 0.138 |
| R-free | 0.18729 |
| Structure solution method | MOLECULAR REPLACEMENT |
| RMSD bond length | 0.023 |
| RMSD bond angle | 2.061 |
| Data reduction software | DENZO |
| Data scaling software | SCALEPACK |
| Phasing software | AMoRE |
| Refinement software | REFMAC (5.8.0069) |
Data quality characteristics
| Overall | Outer shell | |
| Low resolution limit [Å] | 50.000 | 1.240 |
| High resolution limit [Å] | 1.200 | 1.200 |
| Rmerge | 0.078 | 0.563 |
| Number of reflections | 39985 | |
| <I/σ(I)> | 17.99 | 2.29 |
| Completeness [%] | 96.2 | |
| Redundancy | 3 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, SITTING DROP | 8.5 | 277 | BRD4-BD1 protein at 1mM, 2.682 M Formate, 10% Glycerol, 0.1 M Tris-HCL pH 8.5 |
