7G73

Crystal Structure of rat Autotaxin in complex with 6-(4-acetylpiperazin-1-yl)-3-[[1-[(3,4-dichlorophenyl)methyl]triazol-4-yl]methyl]quinazolin-4-one, i.e. SMILES c1(ccc2c(c1)C(=O)N(C=N2)CC1=CN(N=N1)Cc1ccc(c(c1)Cl)Cl)N1CCN(CC1)C(=O)C with IC50=0.0309414 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	84.221, 91.859, 120.559
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	49.020 - 1.520
R-factor	0.1687
Rwork	0.167
R-free	0.19500
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	PHENIX (1.20.1_4487)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	49.020	49.020	1.560
High resolution limit [Å]	1.520	6.800	1.520
Rmerge	0.089	0.026	2.577
Rmeas	0.096	0.029	2.784
Total number of observations	955690
Number of reflections	142156	1807	10317
<I/σ(I)>	12.31	50.56	0.73
Completeness [%]	98.7	99.1	97.4
Redundancy	6.723	6.194	6.894
CC(1/2)	0.999	0.999	0.324

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