5VGO

Bruton's tyrosine kinase (BTK) with compound G-744

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL12-2
Synchrotron site	SSRL
Beamline	BL12-2
Temperature [K]	110
Detector technology	PIXEL
Collection date	2014-06-14
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.9795
Spacegroup name	P 61
Unit cell lengths	108.314, 108.314, 42.570
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	46.901 - 1.621
R-factor	0.1622
Rwork	0.161
R-free	0.18430
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4rx5
RMSD bond length	0.006
RMSD bond angle	1.052
Data reduction software	XDS
Data scaling software	Aimless
Phasing software	REFMAC
Refinement software	PHENIX (1.9_1692)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	46.901	1.680
High resolution limit [Å]	1.620	1.620
Number of reflections	36419	2733
<I/σ(I)>	28.6	2.5
Completeness [%]	99.0	99
Redundancy	10.1	10

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	5.5	286	reservoir 0.1 M LiSO4, 0.1 M citric acid pH 5.5, 6% PEG 10K, 0.4% beta-octylglucoside protein 8 mg/mL 10 mM Tris 8.5, 0.1 M NaCl, 0.5 mM TCEP, G-744 made 0.5 mM using 10 mM DMSO stock drop 1:2 protein/reservoir.