7G33

Crystal Structure of rat Autotaxin in complex with (3,5-dichlorophenyl)methyl 7-(3H-benzotriazole-5-carbonylamino)-5-oxa-2-azaspiro[3.4]octane-2-carboxylate, i.e. SMILES C12(C[C@@H](CO1)NC(=O)c1cc3c(cc1)N=NN3)CN(C2)C(=O)OCc1cc(cc(c1)Cl)Cl with IC50=0.00754101 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	CCD
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	1
Spacegroup name	P 21 21 21
Unit cell lengths	84.176, 91.747, 119.809
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.810 - 1.600
R-factor	0.1868
Rwork	0.185
R-free	0.22150
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.018
RMSD bond angle	1.831
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.7.0029)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	48.810	48.810	1.640
High resolution limit [Å]	1.600	7.160	1.600
Rmerge	0.111	0.034	2.457
Rmeas	0.116	0.035	2.567
Total number of observations	1611199
Number of reflections	122078	1534	8972
<I/σ(I)>	14.35	46.92	1.03
Completeness [%]	100.0	99.3	100
Redundancy	13.198	12.074	11.933
CC(1/2)	0.999	1.000	0.421

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