7G2M

Crystal Structure of rat Autotaxin in complex with 5-fluoro-6-[2-[3-[2-[(5-methyltetrazol-2-yl)methyl]-4-(trifluoromethyl)phenyl]propanoyl]-1,3,4,6-tetrahydropyrrolo[3,4-c]pyrrole-5-carbonyl]pyridine-3-sulfonamide, i.e. SMILES C12=C(CN(C1)C(=O)CCc1ccc(cc1CN1N=NC(=N1)C)C(F)(F)F)CN(C2)C(=O)c1ncc(cc1F)S(=O)(=O)N with IC50=0.0018642 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	2015-12-13
Detector	PSI PILATUS 6M
Wavelength(s)	0.999970
Spacegroup name	P 21 21 21
Unit cell lengths	83.891, 91.227, 119.009
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.530 - 2.410
R-factor	0.1915
Rwork	0.189
R-free	0.24520
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.010
RMSD bond angle	1.383
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0103)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	48.530	48.530	2.470
High resolution limit [Å]	2.410	10.780	2.410
Rmerge	0.084	0.034	0.972
Rmeas	0.091	0.038	1.068
Total number of observations	234831
Number of reflections	35976	473	2621
<I/σ(I)>	15.81	43.51	1.85
Completeness [%]	99.9	97.9	99.2
Redundancy	6.527	5.416	5.818
CC(1/2)	0.999	0.999	0.649

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