7G5G

Crystal Structure of rat Autotaxin in complex with 1-[2-(cyclohexylmethyl)-1,3-dioxoisoindol-4-yl]-N-[(4-methyl-1,2,5-oxadiazol-3-yl)methyl]piperidine-4-carboxamide, i.e. SMILES N1(C(=O)c2c(C1=O)cccc2N1CCC(C(=O)NCC2=NON=C2C)CC1)CC1CCCCC1 with IC50=0.0435744 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	84.292, 91.860, 120.157
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.930 - 1.960
R-factor	0.1692
Rwork	0.166
R-free	0.22450
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.013
RMSD bond angle	1.346
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	PHENIX (dev_1101)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	45.930	45.930	2.010
High resolution limit [Å]	1.960	8.770	1.960
Rmerge	0.163	0.041	1.293
Rmeas	0.177	0.044	1.399
Total number of observations	445687
Number of reflections	67516	869	4920
<I/σ(I)>	8.66	29.57	1.45
Completeness [%]	99.8	98.8	99.5
Redundancy	6.601	6.372	6.839
CC(1/2)	0.995	0.998	0.666

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