7G36

Crystal Structure of rat Autotaxin in complex with 1H-benzotriazol-5-yl-[rac-(1R,2S,6R,7S)-9-[5-cyclopropyl-6-(cyclopropylmethoxy)pyridine-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)c1nc(c(cc1)C1CC1)OCC1CC1 with IC50=0.0606197 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	2013-04-09
Detector	PSI PILATUS 6M
Wavelength(s)	0.999840
Spacegroup name	P 21 21 21
Unit cell lengths	84.279, 91.958, 120.587
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.980 - 1.970
R-factor	0.196
Rwork	0.194
R-free	0.23400
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.012
RMSD bond angle	1.520
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]	45.980	45.980	2.020
High resolution limit [Å]	1.970	8.810	1.970
Rmerge	0.122	0.026	1.286
Rmeas	0.132	0.028	1.390
Total number of observations	447098
Number of reflections	66915	860	4876
<I/σ(I)>	11.65	48.25	1.48
Completeness [%]	99.9	98.7	99.7
Redundancy	6.682	6.285	6.885
CC(1/2)	0.998	1.000	0.612

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