7G6S

Crystal Structure of rat Autotaxin in complex with 6-chloro-3-[5-cyclopropyl-6-(oxan-4-yloxy)pyridin-3-yl]-1H-pyrazolo[3,4-b]pyridine, i.e. SMILES N1=C(c2c(N1)nc(cc2)Cl)c1cc(c(nc1)OC1CCOCC1)C1CC1 with IC50=1.82666 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	2014-02-10
Detector	PSI PILATUS 6M
Wavelength(s)	0.999980
Spacegroup name	P 21 21 21
Unit cell lengths	84.230, 91.611, 119.792
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	42.780 - 1.940
R-factor	0.1885
Rwork	0.186
R-free	0.22860
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.013
RMSD bond angle	1.562
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0048)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	42.780	42.780	1.990
High resolution limit [Å]	1.940	8.680	1.940
Rmerge	0.115	0.025	2.084
Rmeas	0.125	0.028	2.259
Total number of observations	461780
Number of reflections	69299	885	5051
<I/σ(I)>	11.4	49.59	0.89
Completeness [%]	100.0	98.7	100
Redundancy	6.664	5.807	6.744
CC(1/2)	0.998	0.999	0.324

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