4L7D

Structure of keap1 kelch domain with (1S,2R)-2-{[(1S)-5-methyl-1-[(1-oxo-1,3-dihydro-2H-isoindol-2-yl)methyl]-3,4-dihydroisoquinolin-2(1H)-yl]carbonyl}cyclohexanecarboxylic acid

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	DIAMOND BEAMLINE I03
Synchrotron site	Diamond
Beamline	I03
Temperature [K]	100
Detector technology	PIXEL
Collection date	2012-12-13
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.9763
Spacegroup name	P 21 2 21
Unit cell lengths	75.920, 126.000, 130.300
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.020 - 2.250
R-factor	0.25343
Rwork	0.252
R-free	0.27586
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1zgk
RMSD bond length	0.004
RMSD bond angle	0.959
Data reduction software	XDS
Data scaling software	XDS
Phasing software	PHASER
Refinement software	REFMAC (5.7.0032)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	65.600	2.308
High resolution limit [Å]	2.250	2.250
Number of reflections	60047
Completeness [%]	97.6	97.97

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	4.6	296	1 ul of protein at 12 mg/ml in 20 mM Tris-HCl pH 7.5, 5 mM DTT, 5 mM compound 1 + 2 ul of 2.15 M Sodium Acetate , VAPOR DIFFUSION, HANGING DROP, temperature 296K