6DI1

CRYSTAL STRUCTURE OF BTK IN COMPLEX WITH COVALENT FRAGMENT LIGAND

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	OTHER
Synchrotron site	SLS
Beamline	X06SA
Temperature [K]	100
Detector technology	PIXEL
Collection date	2012-09-07
Detector	DECTRIS PILATUS3 X 1M
Wavelength(s)	1
Spacegroup name	P 21 21 2
Unit cell lengths	72.250, 104.170, 38.120
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	25.000 - 1.100
R-factor	0.1738
Rwork	0.173
R-free	0.18610
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.029
RMSD bond angle	2.371
Data scaling software	HKL-2000
Refinement software	REFMAC (5.5.0066)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	25.000	1.130
High resolution limit [Å]	1.100	1.102
Rmeas	0.045	0.216
Number of reflections	113484	15536
<I/σ(I)>	22.36	5.16
Completeness [%]	97.0	83
Redundancy	5.93	3.34
CC(1/2)	0.999	0.963

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP		294	RESERVOIR SOLUTION : 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