5TT7
Discovery of TAK-659, an Orally Available Investigational Inhibitor of Spleen Tyrosine Kinase (SYK)
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | ALS BEAMLINE 5.0.3 |
Synchrotron site | ALS |
Beamline | 5.0.3 |
Temperature [K] | 100 |
Detector technology | CCD |
Collection date | 2009-10-22 |
Detector | ADSC QUANTUM 315r |
Wavelength(s) | 0.9764848 |
Spacegroup name | P 21 21 21 |
Unit cell lengths | 39.815, 85.204, 88.912 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 30.000 - 1.770 |
R-factor | 0.2076 |
Rwork | 0.206 |
R-free | 0.23450 |
Structure solution method | MOLECULAR REPLACEMENT |
RMSD bond length | 0.007 |
RMSD bond angle | 1.150 |
Data reduction software | HKL-2000 |
Data scaling software | HKL-2000 |
Phasing software | MOLREP |
Refinement software | REFMAC (5.8.0103) |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 50.000 | 50.000 | 1.800 |
High resolution limit [Å] | 1.760 | 4.800 | 1.770 |
Rmerge | 0.082 | 0.049 | 0.675 |
Number of reflections | 30241 | ||
<I/σ(I)> | 10.2 | ||
Completeness [%] | 98.9 | 99.9 | 97.2 |
Redundancy | 5.5 | 5.3 | 4.3 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, SITTING DROP | 8.7 | 293 | 1.2M Potassium Na Tartrate, 0.1M Tris pH 8.7 |