7G63

Crystal Structure of rat Autotaxin in complex with [4-cyano-2-(2,2-dimethylpropanoylamino)phenyl]methyl (3aS,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)OCc1c(cc(cc1)C#N)NC(=O)C(C)(C)C with IC50=0.0139432 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	2013-08-23
Detector	PSI PILATUS 6M
Wavelength(s)	0.920200
Spacegroup name	P 21 21 21
Unit cell lengths	84.949, 92.763, 119.159
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.380 - 2.080
R-factor	0.2073
Rwork	0.205
R-free	0.25150
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.011
RMSD bond angle	1.498
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0048)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	46.380	46.380	2.130
High resolution limit [Å]	2.080	9.300	2.080
Rmerge	0.121	0.026	2.362
Rmeas	0.131	0.028	2.569
Total number of observations	379699
Number of reflections	57299	739	4192
<I/σ(I)>	10.93	41.46	0.84
Completeness [%]	100.0	98.5	100
Redundancy	6.627	5.889	6.458
CC(1/2)	0.998	0.999	0.329

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