7G7Q

Crystal Structure of rat Autotaxin in complex with [2-cyclopropyl-6-(oxan-4-ylmethoxy)pyridin-4-yl]-[rac-(3aR,8aS)-2-(3-hydroxy-5,7-dihydro-4H-[1,2]oxazolo[5,4-c]pyridine-6-carbonyl)-1,3,3a,4,5,7,8,8a-octahydropyrrolo[3,4-d]azepin-6-yl]methanone, i.e. SMILES N1(C(=O)N2C[C@H]3CCN(CC[C@H]3C2)C(=O)c2cc(C3CC3)nc(OCC3CCOCC3)c2)CC2=C(CC1)C(=NO2)O with IC50=0.00552809 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	2015-03-08
Detector	PSI PILATUS 6M
Wavelength(s)	0.999990
Spacegroup name	P 21 21 21
Unit cell lengths	83.707, 91.171, 118.333
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.320 - 2.020
R-factor	0.1956
Rwork	0.192
R-free	0.25930
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.017
RMSD bond angle	1.883
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0103)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	48.320	48.320	2.070
High resolution limit [Å]	2.020	9.030	2.020
Rmerge	0.137	0.029	2.586
Rmeas	0.149	0.032	2.800
Total number of observations	396433
Number of reflections	60055	773	4413
<I/σ(I)>	10.19	45.08	0.75
Completeness [%]	99.9	98.3	99.8
Redundancy	6.601	5.768	6.743
CC(1/2)	0.998	0.999	0.307

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