7G2N

Crystal Structure of rat Autotaxin in complex with 5-fluoro-6-[1-[3-[2-[(5-methyltetrazol-2-yl)methyl]-4-(trifluoromethyl)phenyl]propanoyl]piperidin-4-yl]sulfanylpyridine-3-sulfonamide, i.e. SMILES O=C(N1CC[C@@H](Sc2c(F)cc(S(=O)(=O)N)cn2)CC1)CCc1ccc(cc1CN1N=NC(=N1)C)C(F)(F)F with IC50=0.00881095 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	83.952, 91.409, 119.249
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.610 - 2.400
R-factor	0.2015
Rwork	0.199
R-free	0.25880
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.011
RMSD bond angle	1.509
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]	48.610	48.610	2.460
High resolution limit [Å]	2.400	10.730	2.400
Rmerge	0.146	0.025	1.800
Rmeas	0.159	0.028	1.980
Total number of observations	240432
Number of reflections	36603	479	2650
<I/σ(I)>	11.7	49.53	1
Completeness [%]	99.9	98.2	99.9
Redundancy	6.569	5.436	5.79
CC(1/2)	0.997	0.999	0.354

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