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 |