7G6Y

Crystal Structure of rat Autotaxin in complex with 1-[4-[[7-[(3,4-difluorophenyl)methyl]-9-methyl-8-oxopurin-2-yl]amino]benzoyl]piperidine-4-sulfonamide, i.e. SMILES c1nc(nc2c1N(C(=O)N2C)Cc1ccc(c(c1)F)F)Nc1ccc(cc1)C(=O)N1CCC(CC1)S(=O)(=O)N with IC50=0.00233021 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	2014-05-10
Detector	PSI PILATUS 6M
Wavelength(s)	1.000010
Spacegroup name	P 21 21 21
Unit cell lengths	84.007, 92.008, 120.287
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	48.900 - 1.480
R-factor	0.1831
Rwork	0.182
R-free	0.20910
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.017
RMSD bond angle	1.866
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.8.0048)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	48.900	48.900	1.520
High resolution limit [Å]	1.480	6.620	1.480
Rmerge	0.085	0.026	2.001
Rmeas	0.092	0.028	2.159
Total number of observations	1029682
Number of reflections	153568	1932	11113
<I/σ(I)>	12.59	46.96	0.95
Completeness [%]	98.8	99.4	97.7
Redundancy	6.705	6.379	6.975
CC(1/2)	0.999	0.999	0.375

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