6DI5

CRYSTAL STRUCTURE OF BTK IN COMPLEX WITH COVALENT INHIBITOR

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SLS BEAMLINE X10SA
Synchrotron site	SLS
Beamline	X10SA
Temperature [K]	100
Detector technology	PIXEL
Collection date	2013-07-30
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.03300
Spacegroup name	P 21 21 2
Unit cell lengths	74.033, 107.696, 39.320
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	43.550 - 1.420
R-factor	0.1786
Rwork	0.178
R-free	0.19470
RMSD bond length	0.027
RMSD bond angle	1.781
Data scaling software	HKL-2000
Refinement software	REFMAC (5.5.0066)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	1.510
High resolution limit [Å]	1.420	1.420
Rmerge	0.044	0.570
Number of reflections	59227
<I/σ(I)>	23.9	3.21
Completeness [%]	98.4	95.9
Redundancy	6.5	6.48

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP		294	25% PEG 3350, 0.2M AMMONIUM ACETATE, 0.1M HEPES pH 6.9, 3% GLYCEROL PROTEIN SOLUTION : 10 mg/mL IN 20 mM TRIS, 50 mM NaCl, 3 mM DTT, pH 8.0