4L7C

Structure of keap1 kelch domain with 2-{[(1S)-2-{[(1R,2S)-2-(1H-tetrazol-5-yl)cyclohexyl]carbonyl}-1,2,3,4-tetrahydroisoquinolin-1-yl]methyl}-1H-isoindole-1,3(2H)-dione

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SLS BEAMLINE X06DA
Synchrotron site	SLS
Beamline	X06DA
Temperature [K]	100
Detector technology	PIXEL
Collection date	2012-11-22
Detector	DECTRIS PILATUS 2M
Wavelength(s)	1
Spacegroup name	P 21 2 21
Unit cell lengths	76.290, 125.610, 132.630
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	36.660 - 2.400
R-factor	0.26626
Rwork	0.265
R-free	0.28064
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1zgk
RMSD bond length	0.004
RMSD bond angle	0.956
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]	36.710	2.462
High resolution limit [Å]	2.400	2.400
Number of reflections	48009
Completeness [%]	99.9	100

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