7G6M

Crystal Structure of rat Autotaxin in complex with [(3aS,6aS)-5-[2-cyclopropyl-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 N1(C[C@@H]2[C@@H](C1)CN(C2)C(=O)c1cc(nc(c1)OCC1CCOCC1)C1CC1)C(=O)c1ccc2c(c1)N=NN2 with IC50=0.00159445 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	CCD
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	1
Spacegroup name	P 21 21 21
Unit cell lengths	84.691, 92.560, 120.715
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.280 - 2.130
R-factor	0.2169
Rwork	0.214
R-free	0.27100
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.018
RMSD bond angle	2.050
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0048)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	46.280	46.280	2.190
High resolution limit [Å]	2.130	9.530	2.130
Rmerge	0.221	0.051	3.302
Rmeas	0.230	0.054	3.431
Total number of observations	694408
Number of reflections	53718	693	3911
<I/σ(I)>	13	50.11	1.12
Completeness [%]	99.8	98.4	100
Redundancy	12.927	11.183	13.447
CC(1/2)	0.998	0.999	0.458

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