7G53

Crystal Structure of rat Autotaxin in complex with 1H-benzotriazol-5-yl-[rac-(1R,2S,6R,7S)-9-[4-(2-methoxyethoxy)quinoline-2-carbonyl]-4,9-diazatricyclo[5.3.0.02,6]decan-4-yl]methanone, i.e. SMILES N1(C[C@H]2[C@@H](C1)[C@H]1[C@@H]2CN(C1)C(=O)c1ccc2c(c1)N=NN2)C(=O)c1nc2c(c(c1)OCCOC)cccc2 with IC50=0.223388 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	2013-02-08
Detector	PSI PILATUS 6M
Wavelength(s)	1.000000
Spacegroup name	P 21 21 21
Unit cell lengths	84.101, 91.980, 119.696
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.990 - 1.730
R-factor	0.1858
Rwork	0.184
R-free	0.22040
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.016
RMSD bond angle	1.712
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]	45.990	45.990	1.770
High resolution limit [Å]	1.730	7.740	1.730
Rmerge	0.105	0.035	1.316
Rmeas	0.114	0.039	1.435
Total number of observations	647346
Number of reflections	97372	1229	7087
<I/σ(I)>	11.44	38.67	1.32
Completeness [%]	99.9	98.9	99.9
Redundancy	6.648	5.925	6.226
CC(1/2)	0.998	0.999	0.506

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