2G01
Pyrazoloquinolones as Novel, Selective JNK1 inhibitors
Experimental procedure
| 実験手法 | 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 4 |
| Spacegroup name | P 32 2 1 |
| 格子定数 [Å] | 150.622, 150.622, 118.996 |
| 格子定数 [度] | 90.00, 90.00, 120.00 |
精密化法
| 残基 | 19.890 - 3.500 |
| R因子 | 0.286 |
| Rwork | 0.283 |
| R-free | 0.35400 |
| Structure solution method | MOLECULAR REPLACEMENT |
| Starting model (for MR) | 1jnk JNK3 KINASE |
| 結合長の平均二乗偏差(RMSD) [Å] | 0.008 |
| 結合角の平均二乗偏差(RMSD) [度] | 1.400 |
| Data reduction software | SDMS |
| Data scaling software | HKL-2000 |
| Phasing software | CNX |
| Refinement software | CNX (2002) |
Quality characteristics
| Overall | Outer shell | |
| 分解能 [Å] (低) | 20.000 | 3.620 |
| 分解能 [Å] (高) | 3.500 | 3.500 |
| Rmerge_l_obs | 0.065 | 0.365 |
| 独立反射数 | 15793 | |
| <I/σ(I)> | 27.9 | 2.6 |
| 完全性 [%] | 81.7 | 63.7 |
| 冗長性 | 5.8 | 5.3 |
結晶化条件
| 結晶ID | 方法 | pH | 温度 | 溶液条件 |
| 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 2uL well solution over 1 mL of well solution. Well solution: 2.8-3.1 M Ammonium Sulfate, 10-14% glycerol. For Co-crystallization experiment 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 |
