7G3T

Crystal Structure of rat Autotaxin in complex with (2S)-6-chloro-2-[[5-(6-oxa-1-azaspiro[3.3]heptane-1-carbonyl)pyrimidin-2-yl]amino]-2,3-dihydro-1H-indene-4-carbonitrile, i.e. SMILES C1c2cc(cc(C#N)c2C[C@H]1Nc1ncc(cn1)C(=O)N1C2(COC2)CC1)Cl with IC50=0.00758135 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	2018-07-23
Detector	PSI PILATUS 6M
Wavelength(s)	1.00004
Spacegroup name	P 21 21 21
Unit cell lengths	83.770, 91.690, 120.290
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	72.920 - 1.330
R-factor	0.1372
Rwork	0.135
R-free	0.17150
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.012
RMSD bond angle	1.633
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0230)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	72.920	72.920	1.360
High resolution limit [Å]	1.330	5.950	1.330
Rmerge	0.096	0.031	2.214
Rmeas	0.104	0.033	2.369
Total number of observations	1549282
Number of reflections	206305	2591	14646
<I/σ(I)>	10.66	41.37	0.82
Completeness [%]	97.3	98.6	94.2
Redundancy	7.51	7.24	7.817
CC(1/2)	0.999	0.999	0.344

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