7G3D

Crystal Structure of rat Autotaxin in complex with 4-tert-butyl-2-chloro-5-(1H-pyrazolo[3,4-b]pyridin-3-ylmethoxy)benzonitrile, i.e. SMILES CC(C)(C)c1cc(Cl)c(C#N)cc1OCC1=NNc2ncccc12 with IC50=0.0201187 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	2015-12-03
Detector	PSI PILATUS 6M
Wavelength(s)	0.999810
Spacegroup name	P 21 21 21
Unit cell lengths	84.230, 91.790, 119.850
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.830 - 1.880
R-factor	0.1791
Rwork	0.177
R-free	0.21800
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]	48.830	48.830	1.930
High resolution limit [Å]	1.880	8.410	1.880
Rmerge	0.129	0.037	1.851
Rmeas	0.139	0.040	1.996
Total number of observations	562114
Number of reflections	76211	966	5547
<I/σ(I)>	11.09	39.61	1.1
Completeness [%]	99.9	98.9	99.9
Redundancy	7.376	6.645	7.124
CC(1/2)	0.998	0.999	0.412

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