7G7E

Crystal Structure of rat Autotaxin in complex with [4-(trifluoromethoxy)phenyl]methyl (3aR,6aR)-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@@H]2CN(C(=O)OCc3ccc(OC(F)(F)F)cc3)C[C@]2(C1)C with IC50=0.0156721 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	83.962, 91.337, 119.725
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	43.000 - 1.940
R-factor	0.1949
Rwork	0.193
R-free	0.24070
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.014
RMSD bond angle	1.655
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]	43.000	43.000	1.990
High resolution limit [Å]	1.940	8.680	1.940
Rmerge	0.161	0.044	1.956
Rmeas	0.175	0.048	2.122
Total number of observations	459830
Number of reflections	68831	882	5019
<I/σ(I)>	8.94	33.7	0.98
Completeness [%]	99.9	98.9	99.9
Redundancy	6.681	5.789	6.672
CC(1/2)	0.996	0.997	0.359

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