7G7I

Crystal Structure of rat Autotaxin in complex with N-[(3-chloro-4-cyanophenyl)methyl]-2-[6-[1-(2-methoxyacetyl)piperidin-4-yl]-4-oxoquinazolin-3-yl]-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)COC with IC50=0.0120222 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	2015-02-03
Detector	PSI PILATUS 6M
Wavelength(s)	0.999920
Spacegroup name	P 21 21 21
Unit cell lengths	84.903, 92.887, 121.125
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.440 - 1.610
R-factor	0.2149
Rwork	0.213
R-free	0.24200
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.015
RMSD bond angle	1.587
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0103)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	46.440	46.440	1.650
High resolution limit [Å]	1.610	7.200	1.610
Rmerge	0.059	0.029	3.402
Rmeas	0.064	0.032	3.696
Total number of observations	813110
Number of reflections	124282	1559	9081
<I/σ(I)>	15.78	44.56	0.6
Completeness [%]	99.9	99.3	99.9
Redundancy	6.542	6.232	6.563
CC(1/2)	0.999	0.999	0.354

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