7G2L

Crystal Structure of rat Autotaxin in complex with 2-chloro-5-(5-cyclopropyloxy-2-fluorophenyl)-4-(1H-pyrazolo[3,4-c]pyridin-3-ylmethoxy)benzonitrile, i.e. SMILES C1C(C1)Oc1ccc(F)c(c1)c1cc(C#N)c(Cl)cc1OCC1=NNc2cnccc12 with IC50=0.787674 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	2015-12-13
Detector	PSI PILATUS 6M
Wavelength(s)	0.999970
Spacegroup name	P 21 21 21
Unit cell lengths	84.032, 91.704, 119.464
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.850 - 1.900
R-factor	0.1773
Rwork	0.175
R-free	0.21150
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.013
RMSD bond angle	1.601
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]	45.850	45.850	1.950
High resolution limit [Å]	1.900	8.500	1.900
Rmerge	0.107	0.030	1.360
Rmeas	0.116	0.033	1.476
Total number of observations	489569
Number of reflections	73230	938	5270
<I/σ(I)>	12.85	47.2	1.42
Completeness [%]	99.8	98.8	97.9
Redundancy	6.685	5.733	6.591
CC(1/2)	0.998	0.999	0.507

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