7G6X

Crystal Structure of rat Autotaxin in complex with N-[(3,4-dichlorophenyl)methyl]-2-[4-oxo-6-[4-(4-sulfamoylbutanoyl)piperazin-1-yl]quinazolin-3-yl]acetamide, i.e. SMILES NS(=O)(=O)CCCC(=O)N1CCN(c2ccc3c(c2)C(=O)N(C=N3)CC(=O)NCc2ccc(c(c2)Cl)Cl)CC1 with IC50=0.00464057 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	2014-03-29
Detector	PSI PILATUS 6M
Wavelength(s)	1.000050
Spacegroup name	P 21 21 21
Unit cell lengths	84.076, 91.944, 119.761
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.970 - 1.540
R-factor	0.1838
Rwork	0.182
R-free	0.21250
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.017
RMSD bond angle	1.815
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0048)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	45.970	45.970	1.580
High resolution limit [Å]	1.540	6.890	1.540
Rmerge	0.077	0.023	2.073
Rmeas	0.084	0.025	2.249
Total number of observations	908990
Number of reflections	137440	1710	10043
<I/σ(I)>	13.6	52.53	0.84
Completeness [%]	99.9	99	100
Redundancy	6.614	5.749	6.691
CC(1/2)	0.999	0.999	0.345

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