7G4I

Crystal Structure of rat Autotaxin in complex with 1H-benzotriazol-5-yl-[rac-(3aR,6aS)-5-[2-(3,5-dichlorophenyl)ethylsulfonyl]-3,3a,4,5,6,6a-hexahydro-1H-cyclopenta[c]pyrrol-2-yl]methanone, i.e. SMILES c1(ccc2c(c1)N=NN2)C(=O)N1C[C@@H]2[C@H](C1)C[C@H](C2)S(=O)(=O)CCc1cc(cc(c1)Cl)Cl with IC50=0.129444 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	2012-05-05
Detector	PSI PILATUS 6M
Wavelength(s)	0.999970
Spacegroup name	P 21 21 21
Unit cell lengths	84.907, 93.091, 121.363
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.590 - 2.620
R-factor	0.2096
Rwork	0.206
R-free	0.27130
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.009
RMSD bond angle	1.432
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.7.0025)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	46.550	46.590	2.690
High resolution limit [Å]	2.620	11.720	2.620
Rmerge	0.133	0.029	1.513
Rmeas	0.144	0.032	1.645
Total number of observations	194825
Number of reflections	29602	389	2166
<I/σ(I)>	11.22	37.12	1.24
Completeness [%]	99.8	97.2	99.6
Redundancy	6.581	5.645	6.496
CC(1/2)	0.997	1.000	0.573

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