7G5D

Crystal Structure of rat Autotaxin in complex with [(3aR,6aR)-5-(1H-benzotriazole-5-carbonyl)-1,3,3a,4,6,6a-hexahydropyrrolo[3,4-c]pyrrol-2-yl]-[4-(4-chlorophenyl)phenyl]methanone, i.e. SMILES N1(C[C@@H]2[C@@H](C1)CN(C2)C(=O)c1ccc(cc1)c1ccc(cc1)Cl)C(=O)c1ccc2c(c1)N=NN2 with IC50=0.00428865 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	2012-10-28
Detector	PSI PILATUS 6M
Wavelength(s)	0.999860
Spacegroup name	P 21 21 21
Unit cell lengths	84.119, 91.914, 120.253
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.920 - 1.810
R-factor	0.1882
Rwork	0.186
R-free	0.22460
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.013
RMSD bond angle	1.642
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]	48.920	48.920	1.860
High resolution limit [Å]	1.810	8.090	1.810
Rmerge	0.081	0.023	1.499
Rmeas	0.088	0.025	1.625
Total number of observations	565907
Number of reflections	85557	1091	6260
<I/σ(I)>	14.44	50.62	1.32
Completeness [%]	99.9	99	100
Redundancy	6.614	5.876	6.745
CC(1/2)	0.999	0.999	0.482

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