4F08
Discovery and Optimization of C-2 Methyl Imidazo-pyrrolopyridines as Potent and Orally Bioavailable JAK1 Inhibitors with Selectivity over JAK2
Experimental procedure
Experimental method | SINGLE |
Source type | SYNCHROTRON |
Source details | ALS BEAMLINE 5.0.1 |
Synchrotron site | ALS |
Beamline | 5.0.1 |
Temperature [K] | 100 |
Detector technology | CCD |
Collection date | 2010-04-16 |
Detector | ADSC QUANTUM 4 |
Wavelength(s) | 1.0 |
Spacegroup name | P 41 |
Unit cell lengths | 110.923, 110.923, 70.732 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 49.610 - 2.820 |
R-factor | 0.2145 |
Rwork | 0.213 |
R-free | 0.24100 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 2b7a |
Data reduction software | DENZO |
Data scaling software | SCALEPACK |
Phasing software | PHASER |
Refinement software | BUSTER-TNT |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 50.000 | 50.000 | 2.920 |
High resolution limit [Å] | 2.820 | 6.070 | 2.820 |
Rmerge | 0.102 | 0.034 | 0.518 |
Number of reflections | 20873 | ||
<I/σ(I)> | 9.2 | ||
Completeness [%] | 99.8 | 100 | 98.3 |
Redundancy | 5 | 4.9 | 4.4 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 6 | 277 | 0.2 M ammonium acetate, 0.1M sodium citrate pH6, 25% PEG 8000, pH 6.0, VAPOR DIFFUSION, HANGING DROP, temperature 277K |