7G2U

Crystal Structure of rat Autotaxin in complex with [2-[2-cyclopropyl-6-(oxan-4-ylmethoxy)pyridine-4-carbonyl]-1,3-dihydroisoindol-5-yl]-(3-hydroxy-6,7-dihydro-4H-[1,2]oxazolo[4,5-c]pyridin-5-yl)methanone, i.e. SMILES C1C(C1)c1cc(C(=O)N2Cc3c(ccc(c3)C(=O)N3CCC4=C(C3)C(=NO4)O)C2)cc(OCC2CCOCC2)n1 with IC50=0.0102556 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	2016-04-06
Detector	PSI PILATUS 6M
Wavelength(s)	1.000080
Spacegroup name	P 21 21 21
Unit cell lengths	82.656, 90.916, 116.659
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	47.660 - 1.740
R-factor	0.1834
Rwork	0.181
R-free	0.22160
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.021
RMSD bond angle	2.003
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]	47.660	47.660	1.790
High resolution limit [Å]	1.740	7.780	1.740
Rmerge	0.114	0.023	2.637
Rmeas	0.124	0.025	2.857
Total number of observations	598878
Number of reflections	90739	1151	6644
<I/σ(I)>	11.21	53.62	0.78
Completeness [%]	99.9	99.1	99.9
Redundancy	6.6	6.523	6.692
CC(1/2)	0.999	0.999	0.278

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