7G5U

Crystal Structure of rat Autotaxin in complex with [(3aS,6aS)-5-[4-(2,2,2-trifluoroethoxy)quinoline-2-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)c1nc2c(c(c1)OCC(F)(F)F)cccc2)C(=O)c1ccc2c(c1)N=NN2 with IC50=0.0117937 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	2013-06-10
Detector	PSI PILATUS 6M
Wavelength(s)	1.000000
Spacegroup name	P 21 21 21
Unit cell lengths	84.092, 91.713, 119.990
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.860 - 2.060
R-factor	0.2026
Rwork	0.201
R-free	0.24080
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.009
RMSD bond angle	1.316
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.7.0029)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	45.860	45.860	2.110
High resolution limit [Å]	2.060	9.210	2.060
Rmerge	0.142	0.028	1.336
Rmeas	0.154	0.030	1.457
Total number of observations	387601
Number of reflections	58034	747	4168
<I/σ(I)>	9.52	46.25	1.06
Completeness [%]	99.9	98.8	98.8
Redundancy	6.679	5.822	6.044
CC(1/2)	0.997	0.999	0.478

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