5UP3

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	SLS BEAMLINE X06DA
Synchrotron site	SLS
Beamline	X06DA
Temperature [K]	100
Detector technology	PIXEL
Collection date	2014-05-30
Detector	DECTRIS PILATUS 2M-F
Wavelength(s)	1.00
Spacegroup name	P 65 2 2
Unit cell lengths	78.790, 78.790, 431.367
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	30.000 - 2.950
R-factor	0.244
Rwork	0.242
R-free	0.28880
RMSD bond length	0.008
RMSD bond angle	1.303
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	3.000
High resolution limit [Å]	2.950	8.000	2.950
Rmerge	0.177	0.088	0.786
Rmeas	0.185	0.093	0.823
Rpim	0.054	0.030	0.242
Total number of observations	218247
Number of reflections	18017
<I/σ(I)>	5
Completeness [%]	100.0	99.7	100
Redundancy	12.1	9.9	11.3
CC(1/2)		0.998	0.892

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6	277	7% polyethylene glycol 2000 MME , 0.05M Ammonium Sulphate, 0.05M MES, pH 6.0