7G56

Crystal Structure of rat Autotaxin in complex with a dimer of [(2R,4S,5S)-5-ethynyl-1-azabicyclo[2.2.2]octan-2-yl]methyl N-cyclohexylcarbamate, i.e. SMILES O=C(NC1CCCCC1)OC[C@H]2C[C@@H]3CCN2C[C@@H]3C#CC#C[C@H]4CN5CC[C@H]4C[C@@H]5COC(=O)NC6CCCCC6 with IC50=4.47875 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	2012-06-29
Detector	PSI PILATUS 6M
Wavelength(s)	0.999970
Spacegroup name	P 21 21 21
Unit cell lengths	84.493, 92.418, 118.751
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.580 - 1.900
R-factor	0.1938
Rwork	0.192
R-free	0.23330
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.013
RMSD bond angle	1.594
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.7.0025)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	48.580	48.580	1.950
High resolution limit [Å]	1.900	8.500	1.900
Rmerge	0.105	0.029	1.706
Rmeas	0.114	0.032	1.864
Total number of observations	487705
Number of reflections	73914	941	5385
<I/σ(I)>	12.88	46.54	1.27
Completeness [%]	99.9	98.8	100
Redundancy	6.598	6.002	6.196
CC(1/2)	0.999	0.999	0.348

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