3P08

Crystal structure of the human BTK kinase domain

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	2008-11-20
Detector	ADSC QUANTUM 315
Wavelength(s)	1.00
Spacegroup name	P 21 21 21
Unit cell lengths	46.602, 103.493, 117.564
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	47.350 - 2.300
R-factor	0.22776
Rwork	0.222
R-free	0.27791
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1k2p
RMSD bond length	0.009
RMSD bond angle	1.180
Data reduction software	HKL-2000
Data scaling software	SCALEPACK
Phasing software	PHASER
Refinement software	REFMAC (5.2.0019)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.380
High resolution limit [Å]	2.300	2.300
<I/σ(I)>	20.6
Completeness [%]	99.2	98.1
Redundancy	4.7	3.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7	277	equal volumes of well solution (0.2 M Na Malonate pH 7.0, 20% PEG 3350, 3% 6-aminocaproic acid) and protein solution (8 mg/mL in 100 mM NaCl, 10 mM Tris-HCL, pH8.5, 1mM TCEP) , VAPOR DIFFUSION, HANGING DROP, temperature 277K