5VO2

DLK in complex with inhibitor 5-(1-isopropyl-5-(1-(oxetan-3-yl)piperidin-4-yl)-1H-pyrazol-3-yl)-3-(trifluoromethyl)pyridin-2-amine (compound 7)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL7-1
Synchrotron site	SSRL
Beamline	BL7-1
Temperature [K]	100
Detector technology	CCD
Collection date	2012-08-23
Detector	ADSC QUANTUM 315
Wavelength(s)	1
Spacegroup name	P 1 21 1
Unit cell lengths	57.290, 39.463, 60.113
Unit cell angles	90.00, 104.81, 90.00

Refinement procedure

Resolution	35.790 - 2.960
R-factor	0.1743
Rwork	0.170
R-free	0.26370
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	5cen
RMSD bond length	0.009
RMSD bond angle	1.020
Data reduction software	XDS
Data scaling software	SCALA (3.3.20)
Phasing software	PHASER
Refinement software	BUSTER (2.11.5)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	39.463	39.463	3.120
High resolution limit [Å]	2.958	9.350	2.960
Rmerge		0.019	0.312
Rmeas	0.135	0.027	0.409
Rpim	0.071	0.015	0.212
Total number of observations	19858
Number of reflections	5586
<I/σ(I)>	11.5	37.2	2.5
Completeness [%]	99.5	98.1	100
Redundancy	3.6	3.3	3.6

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.7	293	20% PEG 3350, 0.2 M Mg Acetate, 0.1 M Hepes pH 7.7