7ORE

Crystal structure of JNK3 in complex with light-activated covalent inhibitor MR-II-249 with both non-covalent and covalent binding modes (compound 4)

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	2018-07-21
Detector	DECTRIS PILATUS3 6M
Wavelength(s)	0.97950
Spacegroup name	P 21 21 21
Unit cell lengths	52.868, 71.059, 107.456
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	29.650 - 2.180
R-factor	0.2189
Rwork	0.216
R-free	0.27590
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4x21
RMSD bond length	0.007
RMSD bond angle	1.274
Data reduction software	XDS
Data scaling software	Aimless (0.7.2)
Phasing software	PHASER
Refinement software	REFMAC (5.8.0238)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	29.650	29.650	2.300
High resolution limit [Å]	2.180	6.890	2.180
Rmerge	0.101	0.053	0.903
Rmeas	0.118	0.057	1.059
Rpim	0.044	0.022	0.393
Number of reflections	21811	780	3134
<I/σ(I)>	10.6		2.1
Completeness [%]	99.9	99	99.9
Redundancy	7.1	6.3	7.1
CC(1/2)	0.997	0.997	0.876

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.8	277.15	16% medium-molecular weight PEG smears (MMW PEG Smears) and 0.1 M HEPES, pH 7.8