7G7N

Crystal Structure of rat Autotaxin in complex with ethyl 5-(3-bromophenyl)-1H-pyrazole-3-carboxylate, i.e. SMILES C1(=NNC(=C1)c1cc(Br)ccc1)C(=O)OCC with IC50=9.48157 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	2015-03-02
Detector	PSI PILATUS 6M
Wavelength(s)	0.999850
Spacegroup name	P 21 21 21
Unit cell lengths	84.430, 92.143, 119.759
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.840 - 2.310
R-factor	0.1923
Rwork	0.189
R-free	0.25540
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.013
RMSD bond angle	1.632
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]	48.840	48.840	2.370
High resolution limit [Å]	2.310	10.330	2.310
Rmerge	0.166	0.034	2.157
Rmeas	0.180	0.038	2.335
Total number of observations	275780
Number of reflections	41688	539	3038
<I/σ(I)>	9.24	36.72	0.95
Completeness [%]	99.9	97.5	99.9
Redundancy	6.615	6.115	6.755
CC(1/2)	0.996	0.998	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