5V19

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 5.0.2
Synchrotron site	ALS
Beamline	5.0.2
Temperature [K]	100
Detector technology	CCD
Collection date	2014-02-06
Detector	ADSC QUANTUM 315r
Wavelength(s)	1.0
Spacegroup name	P 65 2 2
Unit cell lengths	78.595, 78.595, 433.472
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	30.000 - 3.100
R-factor	0.24
Rwork	0.238
R-free	0.28520
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.008
RMSD bond angle	1.268
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	3.150
High resolution limit [Å]	3.100	8.400	3.100
Rmerge	0.086	0.036	0.745
Rmeas	0.093	0.039	0.799
Rpim	0.035	0.015	0.282
Number of reflections	15419
<I/σ(I)>	11
Completeness [%]	98.8	98.1	100
Redundancy	6.8	5.9	7.4
CC(1/2)		0.999	0.879

Crystallization Conditions

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