7G3J

Crystal Structure of rat Autotaxin in complex with 5-tert-butyl-2-chloro-4-[[1-methyl-5-(6-oxa-1-azaspiro[3.3]heptane-1-carbonyl)imidazol-2-yl]methoxy]benzonitrile, i.e. SMILES Clc1c(C#N)cc(C(C)(C)C)c(c1)OCC1=NC=C(C(=O)N2C3(CC2)COC3)N1C with IC50=0.124297 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	2018-04-28
Detector	PSI PILATUS 6M
Wavelength(s)	1.000010
Spacegroup name	P 21 21 21
Unit cell lengths	83.287, 90.915, 117.703
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	71.950 - 1.990
R-factor	0.1678
Rwork	0.165
R-free	0.21180
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.019
RMSD bond angle	1.938
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]	71.950	71.950	2.040
High resolution limit [Å]	1.990	8.900	1.990
Rmerge	0.145	0.038	2.525
Rmeas	0.156	0.041	2.735
Total number of observations	454974
Number of reflections	62016	801	4516
<I/σ(I)>	10.11	37.09	0.87
Completeness [%]	100.0	99	99.9
Redundancy	7.336	6.983	6.839
CC(1/2)	0.998	0.999	0.301

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