7G76

Crystal Structure of rat Autotaxin in complex with 2-[6-(4-acetylpiperazin-1-yl)-4-oxoquinazolin-3-yl]-N-[(3-chloro-4-cyanophenyl)methyl]-N-methylacetamide, i.e. SMILES O=C(C)N1CCN(CC1)c1ccc2N=CN(CC(=O)N(C)Cc3ccc(c(Cl)c3)C#N)C(=O)c2c1 with IC50=0.036628 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	2014-07-18
Detector	PSI PILATUS 6M
Wavelength(s)	1.000010
Spacegroup name	P 21 21 21
Unit cell lengths	84.251, 92.039, 120.888
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.020 - 1.500
R-factor	0.1863
Rwork	0.185
R-free	0.21590
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.014
RMSD bond angle	1.615
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0049)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	46.020	46.020	1.540
High resolution limit [Å]	1.500	6.710	1.500
Rmerge	0.074	0.024	2.205
Rmeas	0.080	0.026	2.382
Total number of observations	995053
Number of reflections	150117	1871	10964
<I/σ(I)>	13.69	51.15	0.86
Completeness [%]	99.7	99.3	99.3
Redundancy	6.629	6.411	6.863
CC(1/2)	0.999	0.999	0.350

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