4RFY

Crystal structure of BTK kinase domain complexed with 6-(dimethylamino)-2-[2-(hydroxymethyl)-3-[1-methyl-5-[[5-(morpholine-4-carbonyl)-2-pyridyl]amino]-6-oxo-3-pyridyl]phenyl]-3,4-dihydroisoquinolin-1-one

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ALS BEAMLINE 5.0.2
Synchrotron site	ALS
Beamline	5.0.2
Temperature [K]	100
Detector technology	CCD
Detector	ADSC QUANTUM 315r
Wavelength(s)	1.0
Spacegroup name	P 21 21 2
Unit cell lengths	71.805, 107.123, 38.305
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	42.910 - 1.700
R-factor	0.18386
Rwork	0.182
R-free	0.21882
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	4otr
RMSD bond length	0.022
RMSD bond angle	1.927
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	CNS
Refinement software	REFMAC (5.8.0048)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	1.740
High resolution limit [Å]	1.700	1.700
Number of reflections	33099
<I/σ(I)>	11.1	2
Completeness [%]	98.4	95.3
Redundancy	5	4.2

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	8	293	33% PEG3350, 0.1 M HEPES, pH 8.0, VAPOR DIFFUSION, HANGING DROP, temperature 293K