7G44

Crystal Structure of rat Autotaxin in complex with (3,5-dichlorophenyl)methyl rac-(3aR,6aS)-2-(4-sulfamoylbenzoyl)-1,3,3a,4,6,6a-hexahydropyrrolo[3,4-c]pyrrole-5-carboxylate, i.e. SMILES C1N(C[C@H]2[C@@H]1CN(C2)C(=O)c1ccc(cc1)S(=O)(=O)N)C(=O)OCc1cc(cc(c1)Cl)Cl with IC50=0.0573624 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	2012-04-02
Detector	PSI PILATUS 6M
Wavelength(s)	0.999990
Spacegroup name	P 21 21 21
Unit cell lengths	83.798, 91.706, 119.736
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.853 - 1.770
R-factor	0.1905
Rwork	0.189
R-free	0.22590
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.014
RMSD bond angle	1.097
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	PHENIX (dev_1019)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	45.850	45.853	1.820
High resolution limit [Å]	1.770	7.920	1.770
Rmerge	0.148	0.040	1.652
Rmeas	0.161	0.043	1.790
Total number of observations	602884
Number of reflections	90473	1150	6606
<I/σ(I)>	10.37	36.56	1.28
Completeness [%]	99.9	98.9	99.9
Redundancy	6.664	6.348	6.75
CC(1/2)	0.997	0.998	0.444

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