6HM6

CRYSTAL STRUCTURE OF SPLEEN TYROSINE KINASE (SYK) IN COMPLEX WITH A 2-(PYRIDINYLOXYMETHYL)PYRIDINE INHIBITOR

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU FR-E+ SUPERBRIGHT
Temperature [K]	100
Detector technology	CCD
Collection date	2009-07-04
Detector	RIGAKU SATURN A200
Wavelength(s)	1.5418
Spacegroup name	P 1 21 1
Unit cell lengths	39.437, 84.982, 40.277
Unit cell angles	90.00, 100.50, 90.00

Refinement procedure

Resolution	20.000 - 2.100
R-factor	0.2167
Rwork	0.213
R-free	0.29030
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	Other in-house coordinates
RMSD bond length	0.008
RMSD bond angle	1.264
Data reduction software	d*TREK (9.9.3L)
Data scaling software	d*TREK (9.9.3L)
Phasing software	REFMAC
Refinement software	REFMAC (5.8.0189)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	42.490	42.490	2.180
High resolution limit [Å]	2.100	4.520	2.100
Rmerge	0.052	0.032	0.437
Rmeas	0.061	0.038	0.517
Number of reflections	15124	1456	1517
<I/σ(I)>	9.9	32.7	2
Completeness [%]	98.9	93.6	99.9
Redundancy	3.53	3.45	3.47

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.5	293	PEG 1500, HEPES, glycerol, tacsimate.