6XIH
Structure-guided optimization of a novel class of ASK1 inhibitors with increased sp3 character and an exquisite selectivity profile
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | ALS BEAMLINE 5.0.3 |
| Synchrotron site | ALS |
| Beamline | 5.0.3 |
| Temperature [K] | 100 |
| Detector technology | CCD |
| Collection date | 2014-08-22 |
| Detector | ADSC QUANTUM 315r |
| Wavelength(s) | 0.9760 |
| Spacegroup name | P 65 2 2 |
| Unit cell lengths | 78.910, 78.910, 429.705 |
| Unit cell angles | 90.00, 90.00, 120.00 |
Refinement procedure
| Resolution | 30.000 - 2.650 |
| R-factor | 0.2275 |
| Rwork | 0.221 |
| R-free | 0.29170 |
| Structure solution method | MOLECULAR REPLACEMENT |
| Starting model (for MR) | 5usq |
| RMSD bond length | 0.007 |
| RMSD bond angle | 1.568 |
| Data reduction software | HKL-2000 |
| Data scaling software | HKL-2000 |
| Phasing software | PHASER |
| Refinement software | REFMAC (5.8.0257) |
Data quality characteristics
| Overall | Inner shell | Outer shell | |
| Low resolution limit [Å] | 50.000 | 50.000 | 2.680 |
| High resolution limit [Å] | 2.630 | 7.130 | 2.630 |
| Rmerge | 0.109 | 0.032 | |
| Rmeas | 0.115 | 0.034 | |
| Rpim | 0.041 | 0.011 | 0.604 |
| Total number of observations | 261550 | ||
| Number of reflections | 24937 | 1476 | 1167 |
| <I/σ(I)> | 6.4 | ||
| Completeness [%] | 99.9 | 98.7 | 99.7 |
| Redundancy | 10.5 | 9.2 | 10.3 |
| CC(1/2) | 0.999 | 0.668 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, SITTING DROP | 6 | 277 | 6% polyethylene glycol 2000 MME , 20% glycerol, 0.1M MES, pH 6.0 |
