4FZ7

Crystal structure of spleen tyrosine kinase complexed with 6-((1R,2S)-2-Amino-cyclohexylamino)-4-(6-ethyl-pyridin-2-ylamino)-pyridazine-3-carboxylic acid amide

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 31-ID
Synchrotron site	APS
Beamline	31-ID
Temperature [K]	100
Detector technology	CCD
Detector	RAYONIX MX225HE
Wavelength(s)	0.97929
Spacegroup name	P 21 21 21
Unit cell lengths	39.630, 84.977, 88.607
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	42.490 - 1.750
R-factor	0.20243
Rwork	0.200
R-free	0.24963
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	3fqe
RMSD bond length	0.024
RMSD bond angle	1.925
Data reduction software	MOSFLM
Data scaling software	SCALA
Phasing software	CNS
Refinement software	REFMAC (5.5.0109)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	44.300	1.760
High resolution limit [Å]	1.670	1.670
Number of reflections	35561
<I/σ(I)>	11.8	1.4
Completeness [%]	99.9	99.9
Redundancy	6.4	6.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.5	283	28% PEG 4000, 0.2M ammonium sulfate, 0.1M HEPES, pH 7.5, VAPOR DIFFUSION, SITTING DROP, temperature 283K