5LMB

HUMAN SPLEEN TYROSINE KINASE KINASE DOMAIN IN COMPLEX WITH AZANAPHTHYRIDINE INHIBITOR

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID23-1
Synchrotron site	ESRF
Beamline	ID23-1
Temperature [K]	100
Detector technology	CCD
Collection date	2009-03-06
Detector	ADSC QUANTUM 315r
Wavelength(s)	1.0724
Spacegroup name	P 1
Unit cell lengths	39.849, 41.780, 86.991
Unit cell angles	99.81, 90.41, 100.03

Refinement procedure

Resolution	20.000 - 1.950
R-factor	0.1777
Rwork	0.175
R-free	0.22810
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	In-house coordinates
RMSD bond length	0.006
RMSD bond angle	1.190
Data scaling software	SCALA (3.3.1)
Refinement software	REFMAC (5.8.0073)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	42.835	42.835	2.060
High resolution limit [Å]	1.950	6.170	1.950
Rmerge	0.055	0.029	0.400
Number of reflections	37810
<I/σ(I)>	8.5	18.5	1.8
Completeness [%]	95.3	94.6	92.8
Redundancy	1.9	1.9	1.9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6.8	293	PEG1500, HEPES, TACSIMATE, GLYCEROL