7G4C

Crystal Structure of rat Autotaxin in complex with 1H-benzotriazol-5-yl-[rac-(1R,2R,6S,7S)-9-(1-ethyl-4-propan-2-yloxyindole-6-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)c1cc2c(c(c1)OC(C)C)C=CN2CC with IC50=0.0412147 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	2013-03-04
Detector	PSI PILATUS 6M
Wavelength(s)	0.999970
Spacegroup name	P 21 21 21
Unit cell lengths	83.835, 91.673, 118.797
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.840 - 1.640
R-factor	0.1778
Rwork	0.176
R-free	0.20870
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.019
RMSD bond angle	1.876
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]	45.840	45.840	1.680
High resolution limit [Å]	1.640	7.330	1.640
Rmerge	0.080	0.023	1.074
Rmeas	0.087	0.026	1.177
Total number of observations	734016
Number of reflections	112393	1416	8209
<I/σ(I)>	18.07	57.24	1.94
Completeness [%]	99.8	98.7	99.6
Redundancy	6.531	5.695	5.807
CC(1/2)	0.999	0.999	0.654

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