7G3E

Crystal Structure of rat Autotaxin in complex with 5-tert-butyl-2-methyl-4-[[3-(2-oxa-7-azaspiro[4.4]nonane-7-carbonyl)-1H-pyrazol-5-yl]methoxy]benzonitrile, i.e. SMILES Cc1cc(c(cc1C#N)C(C)(C)C)OCC1=CC(=NN1)C(=O)N1CC[C@]2(CCOC2)C1 with IC50=0.00824801 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	2018-03-05
Detector	PSI PILATUS 6M
Wavelength(s)	1.000020
Spacegroup name	P 21 21 21
Unit cell lengths	83.939, 91.590, 120.062
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	72.820 - 1.760
R-factor	0.1757
Rwork	0.174
R-free	0.20660
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.016
RMSD bond angle	1.742
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0189)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	61.880	72.820	1.810
High resolution limit [Å]	1.760	7.870	1.760
Rmerge	0.057	0.024	1.419
Rmeas	0.062	0.026	1.522
Total number of observations	676668
Number of reflections	92319	1179	6749
<I/σ(I)>	17.01	56.62	1.32
Completeness [%]	100.0	99.5	100
Redundancy	7.33	6.907	7.563
CC(1/2)	0.999	0.999	0.530

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