4OT6

Crystal structure of BTK kinase domain complexed with 4-Methanesulfonyl-N-(3-{8-[4-(morpholine-4-carbonyl)-phenylamino]-imidazo[1,2-a]pyrazin-6-yl}-phenyl)-benzamide

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ALS BEAMLINE 5.0.2
Synchrotron site	ALS
Beamline	5.0.2
Temperature [K]	100
Detector technology	CCD
Detector	ADSC QUANTUM 315r
Wavelength(s)	1.0
Spacegroup name	P 21 21 2
Unit cell lengths	71.825, 105.389, 38.240
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	42.490 - 2.050
R-factor	0.21936
Rwork	0.216
R-free	0.27788
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	3pix
RMSD bond length	0.012
RMSD bond angle	1.436
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	CNS
Refinement software	REFMAC (5.8.0048)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	42.490	2.100
High resolution limit [Å]	2.050	2.050
Number of reflections	18568
<I/σ(I)>	4.8	1.81
Completeness [%]	95.7	95.97
Redundancy	4.1	2.5

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	8	293	33% PEG3350, 0.1 M HEPES, pH 8.0, VAPOR DIFFUSION, HANGING DROP, temperature 293K