7G77

Crystal Structure of rat Autotaxin in complex with 2-[6-(1-acetylpiperidin-4-yl)-4-oxoquinazolin-3-yl]-N-[(3-chloro-4-cyanophenyl)methyl]-N-methylacetamide, i.e. SMILES c1(ccc2c(c1)C(=O)N(C=N2)CC(=O)N(Cc1cc(c(cc1)C#N)Cl)C)C1CCN(CC1)C(=O)C with IC50=0.0234152 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	84.279, 92.065, 120.974
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	49.140 - 1.790
R-factor	0.1905
Rwork	0.188
R-free	0.23490
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.014
RMSD bond angle	1.636
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]	49.140	49.140	1.840
High resolution limit [Å]	1.790	8.010	1.790
Rmerge	0.128	0.032	2.183
Rmeas	0.139	0.035	2.361
Total number of observations	592666
Number of reflections	88931	1131	6470
<I/σ(I)>	10.23	37.09	0.9
Completeness [%]	99.6	98.9	98.9
Redundancy	6.664	6.013	6.828
CC(1/2)	0.998	0.999	0.390

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