7G2Q

Crystal Structure of rat Autotaxin in complex with 1-[2-[2-cyclopropyl-6-(oxan-4-ylmethoxy)pyridine-4-carbonyl]-1,3,4,6-tetrahydropyrrolo[3,4-c]pyrrole-5-carbonyl]piperidine-4-sulfonamide, i.e. SMILES N1(C(=O)N2CC3=C(CN(C3)C(=O)c3cc(nc(c3)C3CC3)OCC3CCOCC3)C2)CC[C@@H](CC1)S(=O)(=O)N with IC50=0.00248328 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)	0.999890
Spacegroup name	P 21 21 21
Unit cell lengths	84.089, 91.991, 120.355
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	43.200 - 1.830
R-factor	0.1993
Rwork	0.197
R-free	0.24140
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.013
RMSD bond angle	1.605
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]	42.960	43.200	1.880
High resolution limit [Å]	1.830	8.180	1.830
Rmerge	0.119	0.027	2.267
Rmeas	0.130	0.030	2.458
Total number of observations	518022
Number of reflections	79696	1057	6048
<I/σ(I)>	10.55	39.38	0.77
Completeness [%]	96.0	98.8	99.7
Redundancy	6.5	6.043	6.701
CC(1/2)	0.998	0.999	0.323

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