7G4T

Crystal Structure of rat Autotaxin in complex with (6-bromonaphthalen-2-yl)-[rac-(1R,2R,6S,7S)-9-(1H-benzotriazole-5-carbonyl)-4,9-diazatricyclo[5.3.0.02,6]decan-4-yl]methanone, i.e. SMILES N1(C[C@H]2[C@@H](C1)[C@H]1[C@@H]2CN(C1)C(=O)c1ccc2c(c1)N=NN2)C(=O)c1ccc2c(c1)ccc(c2)Br with IC50=0.127386 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	2012-09-22
Detector	PSI PILATUS 6M
Wavelength(s)	1.000040
Spacegroup name	P 21 21 21
Unit cell lengths	84.003, 91.512, 119.553
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.760 - 1.960
R-factor	0.2065
Rwork	0.204
R-free	0.24480
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.011
RMSD bond angle	1.498
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.7.0032)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	45.760	45.760	2.010
High resolution limit [Å]	1.960	8.770	1.960
Rmerge	0.141	0.055	1.709
Rmeas	0.153	0.060	1.851
Total number of observations	436551
Number of reflections	66774	858	4863
<I/σ(I)>	9.87	30.34	1.27
Completeness [%]	99.8	98.7	99.6
Redundancy	6.538	5.551	6.788
CC(1/2)	0.997	0.996	0.476

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