7G3I

Crystal Structure of rat Autotaxin in complex with (6-methylsulfonyl-1,6-diazaspiro[3.3]heptan-1-yl)-[2-[[3-propan-2-yl-5-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]methanone, i.e. SMILES CC(C)c1cc(cc(c1)OC(F)(F)F)CNc1ncc(cn1)C(=O)N1CCC21CN(C2)S(=O)(=O)C with IC50=0.018213 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	2018-04-09
Detector	PSI PILATUS 6M
Wavelength(s)	0.979070
Spacegroup name	P 21 21 21
Unit cell lengths	83.988, 91.306, 118.107
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	61.810 - 1.840
R-factor	0.1741
Rwork	0.172
R-free	0.21220
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.015
RMSD bond angle	1.684
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0189)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	61.810	61.810	1.890
High resolution limit [Å]	1.840	8.230	1.840
Rmerge	0.120	0.056	2.169
Rmeas	0.129	0.060	2.325
Total number of observations	580926
Number of reflections	79427	1018	5814
<I/σ(I)>	9.66	28.17	0.95
Completeness [%]	99.9	99.1	100
Redundancy	7.314	6.718	7.614
CC(1/2)	0.998	0.997	0.432

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