7G2I

Crystal Structure of rat Autotaxin in complex with 3-fluoro-4-[2-[1-[3-[2-[(5-methyltetrazol-2-yl)methyl]-4-(trifluoromethyl)phenyl]propanoyl]piperidin-4-yl]ethylsulfonyl]benzenesulfonamide, i.e. SMILES c1(S(=O)(=O)CC[C@H]2CCN(C(=O)CCc3c(CN4N=C(C)N=N4)cc(C(F)(F)F)cc3)CC2)ccc(S(=O)(=O)N)cc1F with IC50=0.00184303 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	83.539, 91.509, 118.741
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.390 - 1.600
R-factor	0.1601
Rwork	0.159
R-free	0.18490
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.013
RMSD bond angle	1.614
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]	48.390	48.390	1.640
High resolution limit [Å]	1.600	7.170	1.600
Rmerge	0.052	0.024	0.832
Rmeas	0.056	0.026	0.906
Total number of observations	793834
Number of reflections	119792	1503	8668
<I/σ(I)>	19.96	61.06	2.18
Completeness [%]	99.9	99.1	99.2
Redundancy	6.627	5.93	6.324
CC(1/2)	0.999	0.999	0.729

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