8EJB

Bruton's tyrosine kinase in complex with 3-{[4-(1-acetylpiperidin-4-yl)phenyl]amino}-5-[(3R)-3-(3-methyl-2-oxoimidazolidin-1-yl)piperidin-1-yl]pyrazine-2-carboxamide

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 23-ID-D
Synchrotron site	APS
Beamline	23-ID-D
Temperature [K]	100
Detector technology	PIXEL
Collection date	2018-08-01
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.0
Spacegroup name	P 21 21 21
Unit cell lengths	38.210, 76.240, 105.870
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	52.940 - 1.580
R-factor	0.1692
Rwork	0.168
R-free	0.19100
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3gen
RMSD bond length	0.009
RMSD bond angle	0.954
Data reduction software	XDS
Data scaling software	Aimless
Phasing software	PHASER
Refinement software	PHENIX (1.20.1_4487)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	76.240	1.620
High resolution limit [Å]	1.580	1.580
Rmerge	0.136	1.677
Rmeas	0.146	1.793
Rpim	0.051	0.864
Number of reflections	42996	3068
<I/σ(I)>	10.2	1.3
Completeness [%]	99.4	98.6
Redundancy	7.9	7.9
CC(1/2)	0.998	0.549

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		277	12.5% w/v PEG 1000, 12.5% w/v PEG 3350, 12.5% v/v MPD 0.02 M sodium formate, 0.02 M ammonium acetate, 0.02 M trisodium citrate, 0.02 M sodium potassium l-tartrate, 0.02 M sodium oxamate 0.1 M MES/imidazole pH 6.5