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