8E2M

Bruton's tyrosine kinase (BTK) with compound 13

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	2015-10-26
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.000
Spacegroup name	P 2 21 21
Unit cell lengths	38.155, 72.394, 103.946
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	38.155 - 1.904
R-factor	0.1579
Rwork	0.154
R-free	0.19910
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	Internal Previously Solved BTK Structure
RMSD bond length	0.009
RMSD bond angle	0.870
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	PHASER (2.6.0)
Refinement software	PHENIX (1.10_2155)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	1.930
High resolution limit [Å]	1.900	5.160	1.900
Rmerge	0.124	0.056	0.543
Rmeas	0.141	0.065	0.618
Rpim	0.065	0.031	0.290
Number of reflections	23105	1290	1103
<I/σ(I)>	15.1
Completeness [%]	99.4	99.1	98.4
Redundancy	4.3	3.9	4.1
CC(1/2)		0.996	0.835

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.5	277	25-33% PEG-5000 MME, 100 mM MES pH 6.35-6.75, 200 mM Ammonium Sulfate