7G4U

Crystal Structure of rat Autotaxin in complex with (E)-1-[(3aS,8aR)-2-[(5R)-4,5,6,7-tetrahydro-1H-benzotriazole-5-carbonyl]-1,3,3a,4,5,7,8,8a-octahydropyrrolo[3,4-d]azepin-6-yl]-3-[4-(trifluoromethoxy)phenyl]prop-2-en-1-one, i.e. SMILES C1C[C@@H]2[C@H](CCN1C(=O)/C=C/c1ccc(cc1)OC(F)(F)F)CN(C2)C(=O)[C@@H]1CCC2=C(C1)N=NN2 with IC50=0.0213266 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	2012-08-21
Detector	PSI PILATUS 6M
Wavelength(s)	0.999960
Spacegroup name	P 21 21 21
Unit cell lengths	84.353, 92.640, 120.027
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.320 - 1.770
R-factor	0.1949
Rwork	0.193
R-free	0.23430
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.015
RMSD bond angle	1.688
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.7.0027)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	46.320	46.320	1.820
High resolution limit [Å]	1.770	7.920	1.770
Rmerge	0.113	0.021	1.744
Rmeas	0.123	0.023	1.893
Total number of observations	612524
Number of reflections	92154	1170	6721
<I/σ(I)>	12.54	53.72	1.08
Completeness [%]	99.9	99	99.9
Redundancy	6.647	6.219	6.619
CC(1/2)	0.998	1.000	0.374

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