6HRP

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
Collection date	2011-02-02
Detector	ADSC QUANTUM 315r
Wavelength(s)	1.0
Spacegroup name	P 21 21 2
Unit cell lengths	71.805, 106.969, 38.299
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	38.300 - 1.120
R-factor	0.17486
Rwork	0.174
R-free	0.19243
Structure solution method	FOURIER SYNTHESIS
RMSD bond length	0.026
RMSD bond angle	2.084
Data reduction software	MOSFLM
Data scaling software	SCALA
Phasing software	PHASER
Refinement software	REFMAC (5.5.0072)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	42.870	1.180
High resolution limit [Å]	1.120	1.120
Rmerge	0.047	0.482
Number of reflections	112605	15523
<I/σ(I)>	16.9	2.8
Completeness [%]	99.1	94.9
Redundancy	6.2	5.3

Crystallization Conditions

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