5TT7

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	2009-10-22
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.9764848
Spacegroup name	P 21 21 21
Unit cell lengths	39.815, 85.204, 88.912
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	30.000 - 1.770
R-factor	0.2076
Rwork	0.206
R-free	0.23450
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.007
RMSD bond angle	1.150
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	MOLREP
Refinement software	REFMAC (5.8.0103)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	1.800
High resolution limit [Å]	1.760	4.800	1.770
Rmerge	0.082	0.049	0.675
Number of reflections	30241
<I/σ(I)>	10.2
Completeness [%]	98.9	99.9	97.2
Redundancy	5.5	5.3	4.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	8.7	293	1.2M Potassium Na Tartrate, 0.1M Tris pH 8.7