7G7D

Crystal Structure of rat Autotaxin in complex with 5-[3-oxo-3-[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]propyl]-3H-1,3-oxazol-2-one, i.e. SMILES C1C[C@@H]2[C@H](CCN1C(=O)c1cc(nc(c1)OCC1CCOCC1)C1CC1)CN(C2)C(=O)CCC1=CNC(=O)O1 with IC50=0.0580555 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	2014-12-14
Detector	PSI PILATUS 6M
Wavelength(s)	0.999990
Spacegroup name	P 21 21 21
Unit cell lengths	83.702, 91.424, 118.999
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.710 - 2.060
R-factor	0.1917
Rwork	0.189
R-free	0.23720
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.012
RMSD bond angle	1.561
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]	45.710	45.710	2.110
High resolution limit [Å]	2.060	9.210	2.060
Rmerge	0.116	0.032	2.122
Rmeas	0.126	0.035	2.296
Total number of observations	378340
Number of reflections	57084	737	4152
<I/σ(I)>	10.71	40.52	0.93
Completeness [%]	99.8	98.4	99.7
Redundancy	6.628	5.714	6.803
CC(1/2)	0.998	0.999	0.304

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