7G2F

Crystal Structure of rat Autotaxin in complex with 4-[4-[3-[2-[(5-methyltetrazol-2-yl)methyl]-4-(trifluoromethyl)phenyl]propanoyl]piperazin-1-yl]sulfonylbenzenesulfonamide, i.e. SMILES FC(c1cc(c(CCC(=O)N2CCN(CC2)S(=O)(=O)c2ccc(S(=O)(=O)N)cc2)cc1)CN1N=NC(=N1)C)(F)F with IC50=0.0525995 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	2015-09-05
Detector	PSI PILATUS 6M
Wavelength(s)	0.999990
Spacegroup name	P 21 21 21
Unit cell lengths	83.965, 91.367, 119.735
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.750 - 2.320
R-factor	0.1986
Rwork	0.196
R-free	0.25060
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.010
RMSD bond angle	1.419
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]	48.750	48.750	2.380
High resolution limit [Å]	2.320	10.380	2.320
Rmerge	0.115	0.027	1.827
Rmeas	0.125	0.030	1.977
Total number of observations	269501
Number of reflections	40626	530	2953
<I/σ(I)>	12.1	46.62	1.03
Completeness [%]	99.9	98	100
Redundancy	6.634	5.349	6.85
CC(1/2)	0.998	0.999	0.411

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