7G2Y

Crystal Structure of rat Autotaxin in complex with 2-[(R)-2-[1-[3-[2-[(5-methyltetrazol-2-yl)methyl]-4-(trifluoromethyl)phenyl]propanoyl]piperidin-4-yl]ethylsulfinyl]-1,3-thiazole-5-sulfonamide, i.e. SMILES C1(=NC=C(S(=O)(=O)N)S1)[S@](=O)CC[C@H]1CCN(C(=O)CCc2ccc(C(F)(F)F)cc2CN2N=NC(=N2)C)CC1 with IC50=0.00230987 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	2016-08-06
Detector	PSI PILATUS 6M
Wavelength(s)	1.000010
Spacegroup name	P 21 21 21
Unit cell lengths	83.882, 91.634, 119.543
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.680 - 1.680
R-factor	0.181
Rwork	0.179
R-free	0.21950
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.018
RMSD bond angle	1.824
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0135)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	48.680	48.680	1.720
High resolution limit [Å]	1.680	7.510	1.680
Rmerge	0.097	0.030	2.235
Rmeas	0.105	0.033	2.416
Total number of observations	696001
Number of reflections	104399	1322	7581
<I/σ(I)>	12.58	47.96	0.82
Completeness [%]	99.0	98.7	98.1
Redundancy	6.667	6.083	6.81
CC(1/2)	0.999	0.999	0.375

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