7G5L

Crystal Structure of rat Autotaxin in complex with rac-(3aR,8aS)-6-[rac-(E)-3-[4-(trifluoromethoxy)phenyl]prop-2-enoyl]-N-(1H-triazol-5-ylmethyl)-1,3,3a,4,5,7,8,8a-octahydropyrrolo[3,4-d]azepine-2-carboxamide, i.e. SMILES c1c(ccc(c1)/C=C/C(=O)N1CC[C@@H]2[C@H](CC1)CN(C2)C(=O)NCC1=CN=NN1)OC(F)(F)F with IC50=0.493964 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	2012-06-16
Detector	PSI PILATUS 6M
Wavelength(s)	0.999980
Spacegroup name	P 21 21 21
Unit cell lengths	85.072, 93.744, 121.251
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.870 - 2.510
R-factor	0.2096
Rwork	0.207
R-free	0.26300
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.003
RMSD bond angle	1.028
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0411)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	46.870	46.870	2.580
High resolution limit [Å]	2.510	11.230	2.510
Rmerge	0.184	0.051	1.828
Rmeas	0.200	0.056	1.981
Total number of observations	219984
Number of reflections	33750	450	2451
<I/σ(I)>	9.01	28.71	1.26
Completeness [%]	99.6	97.2	99.6
Redundancy	6.518	5.34	6.776
CC(1/2)	0.995	0.997	0.582

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