7G2W

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]benzenesulfonamide, i.e. SMILES c1(ccc(cc1)C(=O)N1CCC2=C(CC1)NN=C2OCc1c(cc(c(c1)C)Cl)C(C)(C)C)S(=O)(=O)N with IC50=0.0150328 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)	0.999990
Spacegroup name	P 21 21 21
Unit cell lengths	81.950, 90.580, 116.490
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.990 - 1.250
R-factor	0.1341
Rwork	0.132
R-free	0.16890
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.023
RMSD bond angle	2.134
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]	48.990	48.990	1.280
High resolution limit [Å]	1.250	5.590	1.250
Rmerge	0.066	0.022	2.044
Rmeas	0.071	0.024	2.221
Total number of observations	1559621
Number of reflections	235120	2946	16848
<I/σ(I)>	13.72	64.52	0.83
Completeness [%]	98.5	99.6	95.9
Redundancy	6.633	6.627	6.433
CC(1/2)	1.000	0.999	0.331

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