7G54

Crystal Structure of rat Autotaxin in complex with tert-butyl (4aR)-9-(4-chloro-2-fluorophenyl)-5,11-dioxo-2,4,4a,6-tetrahydro-1H-pyrazino[2,1-c][1,4]benzodiazepine-3-carboxylate, i.e. SMILES c1cc(cc(c1c1cc2c(cc1)NC(=O)[C@@H]1N(C2=O)CCN(C1)C(=O)OC(C)(C)C)F)Cl with IC50=0.506839 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	2012-06-16
Detector	PSI PILATUS 6M
Wavelength(s)	0.999980
Spacegroup name	P 21 21 21
Unit cell lengths	85.077, 93.061, 121.586
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	43.490 - 2.380
R-factor	0.2341
Rwork	0.231
R-free	0.29270
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.008
RMSD bond angle	1.284
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.7.0025)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	43.460	43.490	2.440
High resolution limit [Å]	2.380	10.640	2.380
Rmerge	0.163	0.027	1.377
Rmeas	0.184	0.030	1.540
Total number of observations	189519
Number of reflections	38717	506	2852
<I/σ(I)>	8.87	34.76	1.25
Completeness [%]	98.1	96.2	99.8
Redundancy	4.895	4.271	5.097
CC(1/2)	0.993	0.999	0.503

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