8IXS

Methyl and Fluorine Effects in Novel Orally Bioavailable Keap1/Nrf2 PPI Inhibitor for Treatment of Chronic Kidney Disease

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SPRING-8 BEAMLINE BL41XU
Synchrotron site	SPring-8
Beamline	BL41XU
Temperature [K]	100
Detector technology	CCD
Collection date	2014-07-15
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	1.0
Spacegroup name	P 61
Unit cell lengths	103.589, 103.589, 55.190
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	89.710 - 1.480
R-factor	0.1654
Rwork	0.164
R-free	0.19050
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.002
RMSD bond angle	0.592
Data reduction software	XDS
Data scaling software	Aimless
Phasing software	PHASER
Refinement software	PHENIX (1.20_4459)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	89.710	1.520
High resolution limit [Å]	1.480	1.480
Rmerge	0.092	0.913
Rmeas	0.093	0.935
Rpim	0.017	0.193
Number of reflections	56260	3884
<I/σ(I)>	3.9	3.9
Completeness [%]	99.5	93.7
Redundancy	29.2	19.8
CC(1/2)		0.903

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION	7.5	278	6-10mg/mL and crystallized with the solution with 0.1M Na acetate (pH5.0) and 1.5M di-ammonium sulfate or the solution with 0.1M Na acetate (pH5.0), 1.5M di-ammonium, and 0.1-0.15M NaCl