5V24

Structure-based drug design of novel ASK1 inhibitors using a fully integrated lead optimization strategy

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	2014-08-22
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.9760
Spacegroup name	P 65 2 2
Unit cell lengths	78.610, 78.610, 429.785
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	30.000 - 2.500
R-factor	0.2359
Rwork	0.234
R-free	0.26590
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.008
RMSD bond angle	1.309
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Refinement software	REFMAC (5.8.0135)

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	0.065	0.035	0.590
Rmeas	0.072	0.039	0.663
Rpim	0.030	0.017	0.295
Total number of observations	159982
Number of reflections	28407
<I/σ(I)>	12.6
Completeness [%]	98.9	97.1	99.9
Redundancy	5.6	4.9	4.8
CC(1/2)		0.998	0.785

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