5LMA

HUMAN SPLEEN TYROSINE KINASE KINASE DOMAIN IN COMPLEX WITH AZANAPHTHYRIDINE 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	PIXEL
Collection date	2016-02-03
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.97950
Spacegroup name	P 1 21 1
Unit cell lengths	39.175, 87.454, 39.851
Unit cell angles	90.00, 99.64, 90.00

Refinement procedure

Resolution	20.000 - 1.430
R-factor	0.1573
Rwork	0.156
R-free	0.18300
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	In-house coordinates
RMSD bond length	0.006
RMSD bond angle	1.188
Data scaling software	Aimless (0.5.12)
Phasing software	REFMAC
Refinement software	REFMAC (5.8.0073)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	43.730	43.730	1.510
High resolution limit [Å]	1.430	4.520	1.430
Rmerge	0.032	0.028	0.107
Number of reflections	46803
<I/σ(I)>	20.4	39.3	5.7
Completeness [%]	96.0	98.2	85.9
Redundancy	3.1	3.2	2.1
CC(1/2)	0.999	0.998	0.978

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		293	PEG3350, Sodium formate.