5UOX

Structure-Based Design of ASK1 Inhibitors as Potential First-in-Class Agents for Heart Failure

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 24-ID-C
Synchrotron site	APS
Beamline	24-ID-C
Temperature [K]	100
Detector technology	PIXEL
Collection date	2014-06-28
Detector	DECTRIS PILATUS 6M-F
Wavelength(s)	0.9789
Spacegroup name	P 65 2 2
Unit cell lengths	78.544, 78.544, 434.028
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	30.000 - 2.500
R-factor	0.2294
Rwork	0.228
R-free	0.25300
RMSD bond length	0.008
RMSD bond angle	1.152
Data reduction software	DENZO
Data scaling software	HKL-2000
Refinement software	REFMAC (5.7.0025)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	2.540
High resolution limit [Å]	2.500	6.780	2.500
Rmerge	0.082	0.054	0.665
Rmeas	0.087	0.057	0.702
Rpim	0.027	0.019	0.221
Total number of observations	300861
Number of reflections	28981
<I/σ(I)>	6.4
Completeness [%]	99.9	99.5	100
Redundancy	10.4	9	9.9
CC(1/2)		0.998	0.876

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6	277	6% polyethylene glycol 2000 MME ,0.05M Ammonium Sulphate, 0.1M MES, pH 6.0