7G4Q

Crystal Structure of rat Autotaxin in complex with (3-chloro-5-cyanophenyl)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)C#N with IC50=0.729656 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	2012-03-23
Detector	PSI PILATUS 6M
Wavelength(s)	0.999880
Spacegroup name	P 21 21 21
Unit cell lengths	83.950, 91.983, 120.009
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.820 - 1.760
R-factor	0.1816
Rwork	0.179
R-free	0.22430
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.019
RMSD bond angle	2.318
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]	48.820	48.820	1.810
High resolution limit [Å]	1.760	7.870	1.760
Rmerge	0.090	0.025	1.773
Rmeas	0.098	0.027	1.928
Total number of observations	611220
Number of reflections	92587	1172	6780
<I/σ(I)>	15.3	52.66	1.41
Completeness [%]	99.9	98.7	99.6
Redundancy	6.602	6.079	6.604
CC(1/2)	0.999	0.999	0.411

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