2H96
Discovery of Potent, Highly Selective, and Orally Bioavailable Pyridine Carboxamide C-jun NH2-terminal Kinase Inhibitors
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | APS BEAMLINE 17-ID |
| Synchrotron site | APS |
| Beamline | 17-ID |
| Temperature [K] | 110 |
| Detector technology | CCD |
| Collection date | 2004-10-18 |
| Detector | ADSC QUANTUM 210 |
| Spacegroup name | P 32 2 1 |
| Unit cell lengths | 155.660, 155.660, 125.163 |
| Unit cell angles | 90.00, 90.00, 120.00 |
Refinement procedure
| Resolution | 19.970 - 3.000 |
| R-factor | 0.2433 |
| Rwork | 0.225 |
| R-free | 0.27800 |
| Structure solution method | MOLECULAR REPLACEMENT |
| Starting model (for MR) | 2g01 |
| RMSD bond length | 0.008 |
| RMSD bond angle | 1.400 |
| Data reduction software | HKL-2000 |
| Data scaling software | HKL-2000 |
| Phasing software | CNX |
| Refinement software | CNX |
Data quality characteristics
| Overall | Outer shell | |
| Low resolution limit [Å] | 20.000 | 3.110 |
| High resolution limit [Å] | 3.000 | 3.000 |
| Rmerge | 0.094 | 0.754 |
| Number of reflections | 31447 | |
| <I/σ(I)> | 22.5 | 2.2 |
| Completeness [%] | 89.1 | 99.5 |
| Redundancy | 7.2 | 6.8 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | 6.2 | PROTEIN WAS PREINCUBATED WITH THE JIP1 PEPTIDE AT A 5X MOLAR EXCESS. PROTEIN CONCENTRATION 9- 12.6 MG/ML. HANGING DROPS CONSISTED OF 2UL PROTEIN PLUS 2 UL WELL SOLUTION. WELL SOLUTION:2.8-3.1 M AMMONIUM SULFATE, 10- 14% GLYCEROL. FOR CO-CRYSTALLIZATION EXPERIMENT WITH THE COMPOUND, THE COMPOUND WAS DISSOLVED IN DMSO AT 100 MM CONCENTRATION. ALLOW TO INCUBATE FOR AT LEAST AN HOUR ON ICE. SOLUTION WAS SPUN FOR 5 MINUTES AT 2000G PRIOR TO SETTING UP FOR CRYSTALLIZATION, PH 6.2, VAPOR DIFFUSION, HANGING DROP, TEMPERATURE 277.0K, pH 6.20 |
