6HM7

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

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	DIAMOND BEAMLINE I04
Synchrotron site	Diamond
Beamline	I04
Temperature [K]	100
Detector technology	CCD
Collection date	2011-08-10
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.9795
Spacegroup name	P 1 21 1
Unit cell lengths	41.114, 84.892, 40.361
Unit cell angles	90.00, 100.16, 90.00

Refinement procedure

Resolution	20.000 - 1.640
R-factor	0.1739
Rwork	0.172
R-free	0.21010
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	OTHER IN-HOUSE COORDINATES
RMSD bond length	0.009
RMSD bond angle	1.406
Data reduction software	MOSFLM (7.0.6)
Data scaling software	SCALA (3.3.16)
Phasing software	REFMAC
Refinement software	REFMAC (5.8.0189)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	42.446	42.446	1.730
High resolution limit [Å]	1.640	5.190	1.640
Rmerge		0.041	0.491
Rmeas	0.077	0.049	0.575
Rpim	0.040	0.026	0.297
Number of reflections	33320	1076	4846
<I/σ(I)>	11.7	8	1.4
Completeness [%]	99.7	98.7	99.9
Redundancy	3.7	3.6	3.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6.5	293	PEG 3350, bistrispropane, sodium bromide