7G4R

Crystal Structure of rat Autotaxin in complex with (3-chloro-5-methylsulfonylphenyl)methyl rac-(3aR,8aS)-2-(1H-benzotriazole-5-carbonyl)-1,3,3a,4,5,7,8,8a-octahydropyrrolo[3,4-d]azepine-6-carboxylate, i.e. SMILES N1(CC[C@@H]2[C@H](CC1)CN(C2)C(=O)c1ccc2c(c1)N=NN2)C(=O)OCc1cc(cc(c1)Cl)S(=O)(=O)C with IC50=0.00849941 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	2012-04-01
Detector	PSI PILATUS 6M
Wavelength(s)	0.999990
Spacegroup name	P 21 21 21
Unit cell lengths	84.497, 92.960, 120.809
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.480 - 2.090
R-factor	0.1851
Rwork	0.183
R-free	0.22000
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.009
RMSD bond angle	1.118
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	PHENIX (dev_1032)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	46.480	46.480	2.140
High resolution limit [Å]	2.090	9.350	2.090
Rmerge	0.120	0.029	1.591
Rmeas	0.130	0.032	1.729
Total number of observations	376450
Number of reflections	56959	729	4159
<I/σ(I)>	11.75	39.72	1.37
Completeness [%]	99.7	97.7	99.7
Redundancy	6.609	5.981	6.483
CC(1/2)	0.998	0.999	0.492

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