7G2R

Crystal Structure of rat Autotaxin in complex with 7-[2-[2-cyclopropyl-6-(oxan-4-ylmethoxy)pyridine-4-carbonyl]-1,3,4,6-tetrahydropyrrolo[3,4-c]pyrrole-5-carbonyl]-2,5,6,8-tetrahydro-[1,2,4]triazolo[4,3-a]pyrazin-3-one, i.e. SMILES N1(C(=O)N2CC3=C(C2)CN(C3)C(=O)c2cc(OCC3CCOCC3)nc(C3CC3)c2)CC2=NNC(=O)N2CC1 with IC50=0.00627428 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	2016-02-27
Detector	PSI PILATUS 6M
Wavelength(s)	0.999990
Spacegroup name	P 21 21 21
Unit cell lengths	84.185, 91.866, 120.483
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	43.230 - 1.700
R-factor	0.1793
Rwork	0.178
R-free	0.20540
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.015
RMSD bond angle	1.663
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0135)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	42.920	43.230	1.740
High resolution limit [Å]	1.700	7.600	1.700
Rmerge	0.094	0.024	1.411
Rmeas	0.102	0.027	1.533
Total number of observations	683974
Number of reflections	101282	1287	7029
<I/σ(I)>	13.36	50.18	1.15
Completeness [%]	98.1	98	93.3
Redundancy	6.753	5.965	6.422
CC(1/2)	0.999	1.000	0.488

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