7G2T

Crystal Structure of rat Autotaxin in complex with 1H-benzotriazol-5-yl-[3-[(2-tert-butyl-4-chloro-5-methylphenyl)methoxy]-4,5,7,8-tetrahydro-1H-pyrazolo[3,4-d]azepin-6-yl]methanone, i.e. SMILES c12c(cc(cc1)C(=O)N1CCC3=C(CC1)NN=C3OCc1c(cc(c(c1)C)Cl)C(C)(C)C)N=NN2 with IC50=0.295297 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)	1.000080
Spacegroup name	P 21 21 21
Unit cell lengths	82.605, 91.023, 117.171
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.510 - 1.550
R-factor	0.1776
Rwork	0.176
R-free	0.20620
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.018
RMSD bond angle	1.863
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]	45.510	45.510	1.590
High resolution limit [Å]	1.550	6.930	1.550
Rmerge	0.083	0.037	2.176
Rmeas	0.090	0.040	2.355
Total number of observations	852472
Number of reflections	128442	1609	9417
<I/σ(I)>	11.23	38.99	0.83
Completeness [%]	100.0	99.3	99.9
Redundancy	6.637	6.574	6.812
CC(1/2)	0.999	0.999	0.309

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