7G2P

Crystal Structure of rat Autotaxin in complex with 1-[2-[2-cyclopropyl-6-(oxan-4-ylmethoxy)pyridine-4-carbonyl]-1,3,4,6-tetrahydropyrrolo[3,4-c]pyrrole-5-carbonyl]-4-fluoropiperidine-4-sulfonamide, i.e. SMILES F[C@@]1(S(=O)(=O)N)CCN(CC1)C(=O)N1CC2=C(CN(C(=O)c3cc(C4CC4)nc(OCC4CCOCC4)c3)C2)C1 with IC50=0.00217681 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	2016-02-21
Detector	PSI PILATUS 6M
Wavelength(s)	0.999950
Spacegroup name	P 21 21 21
Unit cell lengths	84.393, 91.776, 120.238
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.890 - 1.950
R-factor	0.194
Rwork	0.192
R-free	0.23480
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.014
RMSD bond angle	1.667
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0135)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	45.890	45.890	2.000
High resolution limit [Å]	1.950	8.720	1.950
Rmerge	0.119	0.025	2.237
Rmeas	0.129	0.027	2.420
Total number of observations	460258
Number of reflections	68747	882	5010
<I/σ(I)>	11.12	47.89	0.84
Completeness [%]	99.9	98.9	99.9
Redundancy	6.695	5.797	6.875
CC(1/2)	0.998	0.999	0.299

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