6X3N

Co-structure of BTK kinase domain with L-005085737 inhibitor

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 17-ID
Synchrotron site	APS
Beamline	17-ID
Temperature [K]	100
Detector technology	PIXEL
Collection date	2012-04-13
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1
Spacegroup name	P 21 21 2
Unit cell lengths	72.410, 104.830, 38.100
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	31.470 - 1.950
R-factor	0.215
Rwork	0.214
R-free	0.24170
Structure solution method	FOURIER SYNTHESIS
RMSD bond length	0.010
RMSD bond angle	1.020
Data reduction software	DENZO (2.3.1)
Data scaling software	SCALEPACK
Phasing software	BUSTER-TNT
Refinement software	BUSTER (2.11.2)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	1.980
High resolution limit [Å]	1.950	5.290	1.950
Rmerge	0.086	0.061	0.439
Total number of observations	128974
Number of reflections	21501	1201	1042
<I/σ(I)>	5.4
Completeness [%]	98.3	98.1	96.5
Redundancy	6	5.2	6.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.5	277	0.1M Bis-TRIS pH 6.5, 0.1M NaCl, 15% w/v PEG 20K 5mM TCEP Cl, 4mM (S)-4-(8-amino-3-(1-(4-(dimethylamino)butanoyl)pyrrolidin-2-yl)imidazo[1,5-a]pyrazin-1-yl)-N-(thiazol-2-yl)benzamide