7G4Y

Crystal Structure of rat Autotaxin in complex with 1H-benzotriazol-5-yl-[rac-(1R,2S,6R,7S)-9-[4-propan-2-yloxy-7-(trifluoromethyl)quinoline-2-carbonyl]-4,9-diazatricyclo[5.3.0.02,6]decan-4-yl]methanone, i.e. SMILES N1(C[C@H]2[C@@H](C1)[C@H]1[C@@H]2CN(C1)C(=O)c1ccc2c(c1)N=NN2)C(=O)c1nc2c(c(c1)OC(C)C)ccc(c2)C(F)(F)F with IC50=0.0197138 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	2013-02-08
Detector	PSI PILATUS 6M
Wavelength(s)	1.000000
Spacegroup name	P 21 21 21
Unit cell lengths	83.948, 91.632, 119.854
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.820 - 1.880
R-factor	0.1856
Rwork	0.183
R-free	0.22520
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.013
RMSD bond angle	1.594
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.7.0029)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	45.820	45.820	1.930
High resolution limit [Å]	1.880	8.410	1.880
Rmerge	0.107	0.031	1.523
Rmeas	0.116	0.034	1.649
Total number of observations	505821
Number of reflections	75840	962	5536
<I/σ(I)>	11.93	42	1.32
Completeness [%]	99.9	98.8	99.9
Redundancy	6.67	5.844	6.825
CC(1/2)	0.998	0.999	0.490

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