7G55

Crystal Structure of rat Autotaxin in complex with [3-chloro-5-(trifluoromethoxy)phenyl]methyl rac-(3aR,6aS)-2-(1H-benzotriazole-5-carbonyl)-1,3,3a,4,6,6a-hexahydropyrrolo[3,4-c]pyrrole-5-carboxylate, i.e. SMILES C1N(C[C@@H]2[C@H]1CN(C2)C(=O)c1ccc2c(c1)N=NN2)C(=O)OCc1cc(cc(c1)Cl)OC(F)(F)F with IC50=0.00942633 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	2012-04-01
Detector	PSI PILATUS 6M
Wavelength(s)	0.999990
Spacegroup name	P 21 21 21
Unit cell lengths	84.022, 92.042, 120.659
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.021 - 2.100
R-factor	0.1925
Rwork	0.190
R-free	0.23490
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.013
RMSD bond angle	1.088
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	PHENIX (dev_1019)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	46.020	46.021	2.150
High resolution limit [Å]	2.100	9.390	2.100
Rmerge	0.131	0.040	1.480
Rmeas	0.142	0.044	1.601
Total number of observations	366234
Number of reflections	55304	710	4039
<I/σ(I)>	10.32	33.17	1.31
Completeness [%]	99.9	98.1	99.9
Redundancy	6.622	5.58	6.848
CC(1/2)	0.997	0.998	0.555

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