7G2O

Crystal Structure of rat Autotaxin in complex with [2-cyclopropyl-6-(oxan-4-ylmethoxy)pyridin-4-yl]-[5-(3-hydroxy-5,7-dihydro-4H-[1,2]oxazolo[5,4-c]pyridine-6-carbonyl)-1,3,4,6-tetrahydropyrrolo[3,4-c]pyrrol-2-yl]methanone, i.e. SMILES N1(C(=O)N2CC3=C(C2)CN(C3)C(=O)c2cc(OCC3CCOCC3)nc(C3CC3)c2)CC2=C(CC1)C(=NO2)O with IC50=0.00526079 microM

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SLS BEAMLINE X10SA
Synchrotron site	SLS
Beamline	X10SA
Temperature [K]	100
Detector technology	PIXEL
Collection date	2016-02-11
Detector	PSI PILATUS 6M
Wavelength(s)	1.000030
Spacegroup name	P 21 21 21
Unit cell lengths	84.125, 91.651, 120.236
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	50.270 - 2.060
R-factor	0.203
Rwork	0.201
R-free	0.24880
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.013
RMSD bond angle	1.598
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0135)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.270	50.270	2.110
High resolution limit [Å]	2.060	9.210	2.060
Rmerge	0.150	0.026	2.480
Rmeas	0.163	0.028	2.694
Total number of observations	385105
Number of reflections	58196	748	4245
<I/σ(I)>	10.36	46.34	0.78
Completeness [%]	99.9	98.7	100
Redundancy	6.617	5.698	6.601
CC(1/2)	0.997	0.999	0.276

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	4.5	293	15.3 mg/mL protein in 20mM BICINE/NaOH pH8.5, 150mM NaCl, 0.02% NaN3 mixed 50-70% with 50-30% reservoir consisting of 11-17% PEG3350, 0.1M Na-acetate pH4.5, 0.2M Ca-acetate, total volume 200nL