5CXH

SYK catalytic domain complexed with a potent orally bioavailable thiazole inhibitor

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ALS BEAMLINE 5.0.3
Synchrotron site	ALS
Beamline	5.0.3
Temperature [K]	100
Detector technology	CCD
Collection date	2013-11-21
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.9765
Spacegroup name	P 21 21 21
Unit cell lengths	40.000, 85.343, 90.076
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	39.830 - 1.900
R-factor	0.1761
Rwork	0.175
R-free	0.20520
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.010
RMSD bond angle	0.990
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	REFMAC
Refinement software	BUSTER-TNT (2.11.2)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	1.970
High resolution limit [Å]	1.900	4.090	1.900
Rmerge	0.096	0.053	0.521
Rmeas	0.114	0.062	0.628
Rpim	0.061	0.033	0.345
Total number of observations	79115
Number of reflections	24752
<I/σ(I)>	8.5
Completeness [%]	98.8	98.3	98.9
Redundancy	3.2	3.1	3
CC(1/2)		0.992	0.726

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.3	277	20% PEG3350, 0.2M potassium fluoride, no buffer pH 7.3