7G7V

Crystal Structure of rat Autotaxin in complex with 3-fluoro-4-[4-[3-[2-[(5-methyltetrazol-2-yl)methyl]-4-(trifluoromethyl)phenyl]propanoyl]piperazin-1-yl]benzenesulfonamide, i.e. SMILES C(=O)(N1CCN(CC1)c1c(cc(cc1)S(=O)(=O)N)F)CCc1ccc(cc1CN1N=NC(=N1)C)C(F)(F)F with IC50=0.0757584 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	2015-05-21
Detector	PSI PILATUS 6M
Wavelength(s)	0.999910
Spacegroup name	P 21 21 21
Unit cell lengths	84.307, 92.430, 119.114
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.640 - 1.620
R-factor	0.1817
Rwork	0.180
R-free	0.21540
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.024
RMSD bond angle	2.145
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]	48.640	48.640	1.660
High resolution limit [Å]	1.620	7.240	1.620
Rmerge	0.091	0.033	1.962
Rmeas	0.098	0.036	2.122
Total number of observations	789356
Number of reflections	118601	1496	8664
<I/σ(I)>	11.61	39.09	0.95
Completeness [%]	100.0	99.3	100
Redundancy	6.656	6.492	6.83
CC(1/2)	0.999	0.999	0.360

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