7G5N

Crystal Structure of rat Autotaxin in complex with 1H-benzotriazol-5-yl-[rac-(1R,2R,6S,7S)-9-(4-methoxynaphthalene-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)c1cc(c2c(c1)cccc2)OC with IC50=0.0878229 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	2012-12-09
Detector	PSI PILATUS 6M
Wavelength(s)	0.999980
Spacegroup name	P 21 21 21
Unit cell lengths	83.932, 91.400, 118.690
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.700 - 1.670
R-factor	0.1852
Rwork	0.184
R-free	0.21490
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.015
RMSD bond angle	1.712
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]	45.700	45.700	1.710
High resolution limit [Å]	1.670	7.470	1.670
Rmerge	0.102	0.032	1.670
Rmeas	0.111	0.035	1.809
Total number of observations	704111
Number of reflections	106366	1341	7803
<I/σ(I)>	12.31	41.78	1.24
Completeness [%]	99.9	99.1	99.9
Redundancy	6.62	5.833	6.779
CC(1/2)	0.999	0.999	0.464

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