5UOR

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	ALS BEAMLINE 5.0.3
Synchrotron site	ALS
Beamline	5.0.3
Temperature [K]	100
Detector technology	CCD
Collection date	2014-10-10
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.9765
Spacegroup name	P 65 2 2
Unit cell lengths	78.485, 78.485, 431.659
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	30.000 - 2.750
R-factor	0.2054
Rwork	0.202
R-free	0.26730
RMSD bond length	0.008
RMSD bond angle	1.379
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	2.800
High resolution limit [Å]	2.750	7.460	2.750
Rmerge	0.094	0.030	0.797
Rmeas	0.103	0.034	0.871
Rpim	0.040	0.015	0.331
Total number of observations	124658
Number of reflections	21840
<I/σ(I)>	7.9
Completeness [%]	99.8	97.8	100
Redundancy	5.7	4.9	5.9
CC(1/2)		0.999	0.660

Crystallization Conditions

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