3R22
Design, synthesis, and biological evaluation of pyrazolopyridine-sulfonamides as potent multiple-mitotic kinase (MMK) inhibitors (Part I)
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | APS BEAMLINE 31-ID |
| Synchrotron site | APS |
| Beamline | 31-ID |
| Temperature [K] | 193 |
| Detector technology | CCD |
| Collection date | 2008-06-11 |
| Detector | RAYONIX MX-225 |
| Wavelength(s) | 0.9793 |
| Spacegroup name | P 61 2 2 |
| Unit cell lengths | 81.384, 81.384, 166.393 |
| Unit cell angles | 90.00, 90.00, 120.00 |
Refinement procedure
| Resolution | 40.700 - 2.900 |
| R-factor | 0.27087 |
| Rwork | 0.269 |
| R-free | 0.31298 |
| Structure solution method | MOLECULAR REPLACEMENT |
| Starting model (for MR) | 3fdn |
| RMSD bond length | 0.013 |
| RMSD bond angle | 1.739 |
| Data reduction software | HKL-2000 |
| Data scaling software | HKL-2000 |
| Phasing software | MOLREP |
| Refinement software | REFMAC (5.5.0109) |
Data quality characteristics
| Overall | Outer shell | |
| Low resolution limit [Å] | 50.000 | 3.000 |
| High resolution limit [Å] | 2.900 | 2.900 |
| Rmerge | 0.051 | 0.567 |
| Number of reflections | 7345 | |
| <I/σ(I)> | 50.15 | 4.1 |
| Completeness [%] | 99.8 | 100 |
| Redundancy | 9.8 | 10.6 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, SITTING DROP | 9 | 298 | 10% Peg550 MME, 0.1M Tris pH 9, 10% ethylene glycol, VAPOR DIFFUSION, SITTING DROP, temperature 298K |
