7G30

Crystal Structure of rat Autotaxin in complex with 3-fluoro-4-[[1-[3-[2-[(5-methyltetrazol-2-yl)methyl]-4-(trifluoromethyl)phenyl]propanoyl]piperidin-4-yl]methylsulfanyl]benzenesulfonamide, i.e. SMILES c1(c(F)cc(S(=O)(=O)N)cc1)SC[C@H]1CCN(CC1)C(=O)CCc1ccc(cc1CN1N=NC(=N1)C)C(F)(F)F with IC50=0.0105744 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	2015-10-09
Detector	PSI PILATUS 6M
Wavelength(s)	1.000090
Spacegroup name	P 21 21 21
Unit cell lengths	84.091, 92.158, 120.803
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.080 - 1.880
R-factor	0.1921
Rwork	0.190
R-free	0.22810
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.015
RMSD bond angle	1.740
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]	46.080	46.080	1.930
High resolution limit [Å]	1.880	8.410	1.880
Rmerge	0.112	0.029	1.839
Rmeas	0.120	0.032	1.987
Total number of observations	561697
Number of reflections	76945	976	5602
<I/σ(I)>	11.79	41.57	1.05
Completeness [%]	99.9	98.7	99.4
Redundancy	7.3	6.64	7.002
CC(1/2)	0.998	0.999	0.488

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