7G7B

Crystal Structure of rat Autotaxin in complex with [4-(trifluoromethoxy)phenyl]methyl (3aS,6aS)-3a-methyl-2-(4-sulfamoylbenzoyl)-3,4,6,6a-tetrahydro-1H-pyrrolo[3,4-c]pyrrole-5-carboxylate, i.e. SMILES NS(=O)(=O)c1ccc(cc1)C(=O)N1C[C@]2(CN(C(=O)OCc3ccc(OC(F)(F)F)cc3)C[C@@H]2C1)C with IC50=0.0121906 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	2014-12-14
Detector	PSI PILATUS 6M
Wavelength(s)	0.999990
Spacegroup name	P 21 21 21
Unit cell lengths	83.901, 91.470, 119.860
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.770 - 1.790
R-factor	0.1916
Rwork	0.190
R-free	0.23010
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.013
RMSD bond angle	1.545
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0049)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	48.770	48.770	1.840
High resolution limit [Å]	1.790	8.010	1.790
Rmerge	0.135	0.051	1.969
Rmeas	0.147	0.056	2.128
Total number of observations	584698
Number of reflections	87397	1110	6374
<I/σ(I)>	8.28	25.85	0.86
Completeness [%]	99.9	98.4	99.9
Redundancy	6.69	5.923	6.846
CC(1/2)	0.997	0.997	0.390

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