7G6K

Crystal Structure of rat Autotaxin in complex with [4-(trifluoromethoxy)phenyl]methyl (3aS,6aS)-2-(2-oxo-1H-[1,3]oxazolo[5,4-b]pyridine-5-carbonyl)-1,3,3a,4,6,6a-hexahydropyrrolo[3,4-c]pyrrole-5-carboxylate, i.e. SMILES C1N(C[C@@H]2[C@@H]1CN(C2)C(=O)OCc1ccc(cc1)OC(F)(F)F)C(=O)c1ccc2c(n1)OC(=O)N2 with IC50=0.00908453 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	2014-02-11
Detector	PSI PILATUS 6M
Wavelength(s)	0.999950
Spacegroup name	P 21 21 21
Unit cell lengths	84.689, 92.202, 121.149
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	49.270 - 2.290
R-factor	0.1979
Rwork	0.195
R-free	0.24400
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.008
RMSD bond angle	1.195
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]	49.270	49.270	2.350
High resolution limit [Å]	2.290	10.240	2.290
Rmerge	0.146	0.040	1.827
Rmeas	0.159	0.044	1.991
Total number of observations	285234
Number of reflections	43429	567	3161
<I/σ(I)>	9.66	30.82	1.12
Completeness [%]	99.9	98.1	100
Redundancy	6.568	5.656	6.327
CC(1/2)	0.996	0.998	0.388

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