7G7F

Crystal Structure of rat Autotaxin in complex with 1H-benzotriazol-5-yl-[rac-(3aR,8aS)-6-[2-cyclopropyl-6-(oxan-4-ylmethoxy)pyridine-4-carbonyl]-1,3,3a,4,5,7,8,8a-octahydropyrrolo[3,4-d]azepin-2-yl]methanone, i.e. SMILES C1C[C@@H]2[C@H](CCN1C(=O)c1cc(nc(c1)OCC1CCOCC1)C1CC1)CN(C2)C(=O)c1ccc2c(c1)N=NN2 with IC50=0.00129469 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	2015-03-21
Detector	PSI PILATUS 6M
Wavelength(s)	0.999980
Spacegroup name	P 21 21 21
Unit cell lengths	84.009, 91.379, 119.499
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.690 - 1.960
R-factor	0.1887
Rwork	0.186
R-free	0.23060
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.014
RMSD bond angle	1.692
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]	48.690	48.690	2.010
High resolution limit [Å]	1.960	8.770	1.960
Rmerge	0.113	0.027	2.263
Rmeas	0.123	0.030	2.449
Total number of observations	444440
Number of reflections	66745	859	4868
<I/σ(I)>	12.02	46.03	0.98
Completeness [%]	100.0	98.8	99.9
Redundancy	6.659	5.909	6.876
CC(1/2)	0.998	0.999	0.353

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