7G5P

Crystal Structure of rat Autotaxin in complex with N-[(1R,3S)-3-[(2S)-2-benzyl-4-[2-(methylamino)-2-oxoethyl]-3-oxopiperazine-1-carbonyl]cyclopentyl]-4-chloro-3-(trifluoromethyl)benzamide, i.e. SMILES C1[C@@H](CC[C@@H]1C(=O)N1CCN(C(=O)[C@@H]1Cc1ccccc1)CC(=O)NC)NC(=O)c1ccc(c(c1)C(F)(F)F)Cl with IC50=0.17269 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	2013-05-04
Detector	PSI PILATUS 6M
Wavelength(s)	0.999960
Spacegroup name	P 21 21 21
Unit cell lengths	84.203, 92.065, 119.910
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.030 - 1.570
R-factor	0.1867
Rwork	0.185
R-free	0.21480
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.014
RMSD bond angle	1.623
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.7.0029)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	46.030	46.030	1.610
High resolution limit [Å]	1.570	7.020	1.570
Rmerge	0.104	0.028	1.701
Rmeas	0.113	0.030	1.841
Total number of observations	861080
Number of reflections	129822	1623	9458
<I/σ(I)>	11.88	44.86	1.05
Completeness [%]	99.5	98.6	99.1
Redundancy	6.633	6.17	6.703
CC(1/2)	0.999	0.999	0.447

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