5K5N
Crystal structure of GSK-3beta complexed with PF-04802367, a highly selective brain-penetrant kinase inhibitor
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | APS BEAMLINE 17-BM |
Synchrotron site | APS |
Beamline | 17-BM |
Temperature [K] | 93 |
Detector technology | CCD |
Collection date | 2008-02-20 |
Detector | ADSC QUANTUM 315 |
Wavelength(s) | 1.00 |
Spacegroup name | P 1 21 1 |
Unit cell lengths | 66.293, 99.907, 66.910 |
Unit cell angles | 90.00, 102.90, 90.00 |
Refinement procedure
Resolution | 27.030 - 2.200 |
R-factor | 0.2051 |
Rwork | 0.204 |
R-free | 0.22870 |
Structure solution method | FOURIER SYNTHESIS |
RMSD bond length | 0.009 |
RMSD bond angle | 0.990 |
Data reduction software | DENZO |
Data scaling software | SCALEPACK |
Phasing software | REFMAC |
Refinement software | BUSTER (2.11.6) |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 50.000 | 50.000 | 2.210 |
High resolution limit [Å] | 2.150 | 4.920 | 2.150 |
Rmerge | 0.040 | 0.466 | |
Number of reflections | 44180 | ||
<I/σ(I)> | 11 | ||
Completeness [%] | 95.0 | 98 | 60.6 |
Redundancy | 3.9 | 4.1 | 2.5 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 6.5 | 295 | Protein storage conditions: 20 mM Tris pH 7.8, 5% (v/v) glycerol, 200 mM NaCl, 1 mM TCEP, 0.5 mM EDTA, 0.5% DMSO, and 0.2 mM PF-4802367, Well solution: 18-23% (w/v) PEG MME 5000, 100-150 mM ammonium sulfate, and 100 mM MES pH 6.5, Crystallization set-up: 0.5 + 0.5 uL drops over a well-solution of 200 uL |