2X8E
Discovery of a Novel Class of triazolones as Checkpoint Kinase Inhibitors - Hit to Lead Exploration
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | EMBL/DESY, HAMBURG BEAMLINE X13 |
| Synchrotron site | EMBL/DESY, HAMBURG |
| Beamline | X13 |
| Temperature [K] | 100 |
| Detector technology | CCD |
| Collection date | 2002-11-23 |
| Detector | MARRESEARCH SX-165 |
| Spacegroup name | P 1 21 1 |
| Unit cell lengths | 45.055, 65.858, 54.468 |
| Unit cell angles | 90.00, 101.73, 90.00 |
Refinement procedure
| Resolution | 16.510 - 2.500 |
| R-factor | 0.23547 |
| Rwork | 0.232 |
| R-free | 0.30865 |
| Structure solution method | MOLECULAR REPLACEMENT |
| Starting model (for MR) | 2x8d |
| RMSD bond length | 0.011 |
| RMSD bond angle | 1.531 |
| Data reduction software | MOSFLM |
| Data scaling software | SCALA |
| Phasing software | AMoRE |
| Refinement software | REFMAC (5.5.0102) |
Data quality characteristics
| Overall | Outer shell | |
| Low resolution limit [Å] | 16.550 | 2.640 |
| High resolution limit [Å] | 2.500 | 2.500 |
| Rmerge | 0.110 | 0.270 |
| Number of reflections | 7559 | |
| <I/σ(I)> | 5.4 | 2 |
| Completeness [%] | 72.5 | 26.3 |
| Redundancy | 2.6 | 1.7 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, HANGING DROP | 6.5 | HANGING DROP 3UL PLUS 3UL PROTEIN: 7 MG/ML, 25MM TRIS PH7.5, 500MM NACL, 5% GLYCEROL, 5MM DTT, 2MM COMPOUND WELL: 12-16% (W/V) PEG3350, 100-200MM AMMONIUM SULPHATE, 2% (V/V) GLYCEROL AND 100 MM SODIUM CACODYLATE PH 6.5 |
