7G7K

Crystal Structure of rat Autotaxin in complex with N-[(3-chloro-4-cyanophenyl)methyl]-N-methyl-2-[6-[1-(oxetane-2-carbonyl)piperidin-4-yl]-4-oxoquinazolin-3-yl]acetamide, i.e. SMILES c1(ccc2c(c1)C(=O)N(C=N2)CC(=O)N(Cc1cc(c(cc1)C#N)Cl)C)[C@H]1CCN(CC1)C(=O)[C@H]1OCC1 with IC50=0.0239157 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)	0.999930
Spacegroup name	P 21 21 21
Unit cell lengths	84.080, 92.048, 120.021
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.020 - 1.670
R-factor	0.1942
Rwork	0.192
R-free	0.23000
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.018
RMSD bond angle	1.857
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]	46.020	46.020	1.710
High resolution limit [Å]	1.670	7.470	1.670
Rmerge	0.084	0.026	2.773
Rmeas	0.092	0.028	3.014
Total number of observations	716668
Number of reflections	108445	1374	7940
<I/σ(I)>	12.45	45.36	0.66
Completeness [%]	99.9	99.1	99.9
Redundancy	6.609	6.175	6.529
CC(1/2)	0.999	0.999	0.318

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