7G4N

Crystal Structure of rat Autotaxin in complex with [4-(trifluoromethoxy)phenyl]methyl (3aS,6aS)-2-(6-sulfamoylpyridine-3-carbonyl)-1,3,3a,4,6,6a-hexahydropyrrolo[3,4-c]pyrrole-5-carboxylate, i.e. SMILES FC(Oc1ccc(cc1)COC(=O)N1C[C@H]2[C@H](C1)CN(C2)C(=O)c1cnc(cc1)S(=O)(=O)N)(F)F with IC50=0.0134798 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	2013-03-04
Detector	PSI PILATUS 6M
Wavelength(s)	0.999970
Spacegroup name	P 21 21 21
Unit cell lengths	83.726, 91.477, 118.973
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.740 - 1.670
R-factor	0.1814
Rwork	0.180
R-free	0.21530
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.017
RMSD bond angle	1.746
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.7.0029)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	45.740	45.740	1.710
High resolution limit [Å]	1.670	7.470	1.670
Rmerge	0.095	0.026	1.691
Rmeas	0.103	0.029	1.833
Total number of observations	710323
Number of reflections	106445	1344	7760
<I/σ(I)>	13.16	49	1.15
Completeness [%]	100.0	99.3	100
Redundancy	6.673	5.964	6.742
CC(1/2)	0.999	0.999	0.406

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