7G2H

Crystal Structure of rat Autotaxin in complex with 3-fluoro-4-[1-[3-[2-[(5-methyltetrazol-2-yl)methyl]-4-(trifluoromethyl)phenyl]propanoyl]piperidin-4-yl]sulfonylbenzenesulfonamide, i.e. SMILES O=C(N1CC[C@@H](S(=O)(=O)c2c(F)cc(S(=O)(=O)N)cc2)CC1)CCc1ccc(cc1CN1N=NC(=N1)C)C(F)(F)F with IC50=0.00379624 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	2015-10-05
Detector	PSI PILATUS 6M
Wavelength(s)	0.999980
Spacegroup name	P 21 21 21
Unit cell lengths	83.802, 91.466, 118.707
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.440 - 2.540
R-factor	0.1928
Rwork	0.189
R-free	0.25660
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.013
RMSD bond angle	1.621
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]	48.440	48.440	2.610
High resolution limit [Å]	2.540	11.360	2.540
Rmerge	0.159	0.050	2.384
Rmeas	0.173	0.055	2.592
Total number of observations	202179
Number of reflections	30789	410	2209
<I/σ(I)>	9.52	31.69	0.84
Completeness [%]	99.9	97.9	100
Redundancy	6.567	5.483	6.536
CC(1/2)	0.996	0.996	0.287

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