5TR6

Discovery of TAK-659, an Orally Available Investigational Inhibitor of Spleen Tyrosine Kinase (SYK)

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	2010-07-14
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.9764848
Spacegroup name	P 21 21 21
Unit cell lengths	39.941, 85.283, 90.283
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	30.000 - 1.930
R-factor	0.1945
Rwork	0.193
R-free	0.21720
RMSD bond length	0.007
RMSD bond angle	1.121
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	MOLREP
Refinement software	REFMAC (5.8.0103)

Data quality characteristics

	Overall
Low resolution limit [Å]	50.000
High resolution limit [Å]	1.930
Number of reflections	22613
<I/σ(I)>	17.6
Completeness [%]	99.5
Redundancy	5.1

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6.1	293	0.7M Potassium Na Tartrate, 0.06M MES_Na, 0.04M MES