7G4B

Crystal Structure of rat Autotaxin in complex with [2-fluoro-4-(trifluoromethyl)phenyl]methyl 2-(4,5,6,7-tetrahydro-1H-benzotriazole-5-carbonyl)-2,7-diazaspiro[3.5]nonane-7-carboxylate, i.e. SMILES C1N(CC21CCN(CC2)C(=O)OCc1c(cc(cc1)C(F)(F)F)F)C(=O)[C@H]1CCC2=C(C1)N=NN2 with IC50=0.103944 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	2013-02-21
Detector	PSI PILATUS 6M
Wavelength(s)	0.999970
Spacegroup name	P 21 21 21
Unit cell lengths	84.398, 91.995, 120.378
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	49.000 - 2.160
R-factor	0.2002
Rwork	0.198
R-free	0.24290
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.010
RMSD bond angle	1.370
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]	49.000	49.000	2.220
High resolution limit [Å]	2.160	9.660	2.160
Rmerge	0.140	0.039	1.497
Rmeas	0.153	0.043	1.625
Total number of observations	330152
Number of reflections	50975	662	3696
<I/σ(I)>	9.96	37.7	1.35
Completeness [%]	99.9	98.5	99.8
Redundancy	6.477	5.745	6.58
CC(1/2)	0.997	0.998	0.518

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