7G2V

Crystal Structure of rat Autotaxin in complex with 4-[3-[(2-tert-butyl-4-chloro-5-methylphenyl)methoxy]-4,5,7,8-tetrahydro-1H-pyrazolo[3,4-d]azepine-6-carbonyl]-2,3-difluorobenzenesulfonamide, i.e. SMILES c1(c(c(c(cc1)C(=O)N1CCC2=C(CC1)NN=C2OCc1c(cc(c(c1)C)Cl)C(C)(C)C)F)F)S(=O)(=O)N with IC50=0.0130576 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	2016-04-06
Detector	PSI PILATUS 6M
Wavelength(s)	1.000000
Spacegroup name	P 21 21 21
Unit cell lengths	83.815, 91.549, 119.348
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.610 - 1.520
R-factor	0.1819
Rwork	0.180
R-free	0.21220
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.019
RMSD bond angle	1.904
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0135)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	48.610	48.610	1.560
High resolution limit [Å]	1.520	6.800	1.520
Rmerge	0.060	0.020	2.219
Rmeas	0.066	0.022	2.402
Total number of observations	937001
Number of reflections	140821	1762	10201
<I/σ(I)>	15.32	66.03	0.76
Completeness [%]	99.6	98.8	99
Redundancy	6.654	6.358	6.693
CC(1/2)	0.999	0.999	0.319

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