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 |