5CY3

SYK catalytic domain complexed with a potent and orally bioavailable benzisothiazole 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	2014-04-17
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.9765
Spacegroup name	P 1 21 1
Unit cell lengths	41.504, 37.656, 90.888
Unit cell angles	90.00, 100.14, 90.00

Refinement procedure

Resolution	39.910 - 1.760
R-factor	0.1711
Rwork	0.170
R-free	0.19470
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.010
RMSD bond angle	0.950
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	REFMAC
Refinement software	BUSTER-TNT (2.11.5)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	1.790
High resolution limit [Å]	1.750	4.320	1.750
Rmerge	0.041	0.026	0.414
Rmeas	0.052	0.033	0.523
Rpim	0.031	0.020	0.315
Total number of observations	72734
Number of reflections	27534
<I/σ(I)>	12.4
Completeness [%]	98.9	97.4	98.3
Redundancy	2.6	2.6	2.5
CC(1/2)		0.997	0.800

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.1	293	PEG 3350 20%, ammonium acetate 0.2M