2GMX
Selective Aminopyridine-Based C-Jun N-terminal Kinase inhibitors with cellular activity
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 |
| Wavelength(s) | 1.000 |
| Spacegroup name | P 32 2 1 |
| Unit cell lengths | 150.786, 150.786, 118.660 |
| Unit cell angles | 90.00, 90.00, 120.00 |
Refinement procedure
| Resolution | 19.910 - 3.500 |
| R-factor | 0.278 |
| Rwork | 0.266 |
| R-free | 0.35100 |
| Structure solution method | MOLECULAR REPLACEMENT |
| Starting model (for MR) | 2g01 |
| RMSD bond length | 0.008 |
| RMSD bond angle | 1.500 |
| Data scaling software | HKL-2000 |
| Phasing software | CNX |
| Refinement software | CNX (2002) |
Data quality characteristics
| Overall | Outer shell | |
| Low resolution limit [Å] | 20.000 | 3.620 |
| High resolution limit [Å] | 3.500 | 3.500 |
| Rmerge | 0.078 | 0.385 |
| Number of reflections | 17550 | |
| <I/σ(I)> | 21 | 4.62 |
| Completeness [%] | 87.7 | 99.3 |
| Redundancy | 5.6 | 5.8 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, HANGING DROP | 6.2 | 277 | 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 |
