8S98

Crystal structure of the TYK2 pseudokinase domain in complex with compound 8

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SLS BEAMLINE X10SA
Synchrotron site	SLS
Beamline	X10SA
Temperature [K]	100
Detector technology	PIXEL
Collection date	2017-10-20
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.0000
Spacegroup name	P 21 21 21
Unit cell lengths	48.108, 112.602, 156.856
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	47.470 - 1.870
R-factor	0.22617
Rwork	0.225
R-free	0.27367
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.012
RMSD bond angle	1.778
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0267)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	91.470	2.120
High resolution limit [Å]	1.870	1.870
Rmeas	0.149	0.504
Number of reflections	68019	21481
<I/σ(I)>	10.92	3.55
Completeness [%]	95.2	97.2
Redundancy	4.3	4.1

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP		298	The purified protein was used in crystallization trials employing both, a standard screen with approximately 1200 different conditions, as well as crystallization conditions identified using literature data. Conditions initially obtained have been optimised using standard strategies, systematically varying parameters critically influencing crystallization, such as temperature, protein concentration, drop ratio, and others. These conditions were also refined by systematically varying pH or precipitant concentrations.