7G70

Crystal Structure of rat Autotaxin in complex with [(3aS,6aS)-5-[2-(dimethylamino)-6-(oxan-4-ylmethoxy)pyridine-4-carbonyl]-1,3,3a,4,6,6a-hexahydropyrrolo[3,4-c]pyrrol-2-yl]-(1H-benzotriazol-5-yl)methanone, i.e. SMILES c1(ccc2c(c1)N=NN2)C(=O)N1C[C@@H]2[C@@H](C1)CN(C2)C(=O)c1cc(nc(c1)OCC1CCOCC1)N(C)C with IC50=0.0094279 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	2014-06-09
Detector	PSI PILATUS 6M
Wavelength(s)	0.999870
Spacegroup name	P 21 21 21
Unit cell lengths	84.438, 92.042, 120.427
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.020 - 1.790
R-factor	0.2067
Rwork	0.205
R-free	0.24040
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.012
RMSD bond angle	1.569
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]	43.270	46.020	1.840
High resolution limit [Å]	1.790	8.010	1.790
Rmerge	0.138	0.053	2.436
Rmeas	0.150	0.058	2.631
Total number of observations	594656
Number of reflections	88996	1132	6514
<I/σ(I)>	8.82	30.85	0.77
Completeness [%]	99.9	99.1	100
Redundancy	6.682	6.269	6.911
CC(1/2)	0.997	0.996	0.291

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