7G2S

Crystal Structure of rat Autotaxin in complex with 4-[2-oxo-2-[4-[[4-(trifluoromethyl)phenyl]methyl]-7,8-dihydro-5H-pyrido[4,3-d]pyrimidin-6-yl]ethyl]sulfanylbenzenesulfonamide, i.e. SMILES c1(C(F)(F)F)ccc(Cc2c3CN(C(=O)CSc4ccc(S(=O)(=O)N)cc4)CCc3ncn2)cc1 with IC50=3.44948 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	2016-03-14
Detector	PSI PILATUS 6M
Wavelength(s)	1.000040
Spacegroup name	P 21 21 21
Unit cell lengths	84.010, 91.702, 119.881
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.790 - 1.650
R-factor	0.2184
Rwork	0.216
R-free	0.26270
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.017
RMSD bond angle	1.802
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]	48.790	48.790	1.690
High resolution limit [Å]	1.650	7.380	1.650
Rmerge	0.115	0.034	2.188
Rmeas	0.125	0.037	2.359
Total number of observations	708346
Number of reflections	109042	1394	7879
<I/σ(I)>	12.11	39.26	1.22
Completeness [%]	97.5	97.8	96.2
Redundancy	6.496	5.867	7.092
CC(1/2)	0.998	0.998	0.395

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