7G5J

Crystal Structure of rat Autotaxin in complex with (7E)-7-[(4-bromophenyl)methylidene]-12H-isoquinolino[2,3-a]quinazolin-5-one, i.e. SMILES N12C(=NC(=O)c3c1cccc3)/C(=C/c1ccc(cc1)Br)/c1c(C2)cccc1 with IC50=0.173306 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	2012-06-29
Detector	PSI PILATUS 6M
Wavelength(s)	0.999970
Spacegroup name	P 21 21 21
Unit cell lengths	84.623, 91.903, 120.202
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.950 - 2.180
R-factor	0.2088
Rwork	0.206
R-free	0.26720
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
RMSD bond length	0.010
RMSD bond angle	1.454
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	REFMAC (5.7.0027)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	45.950	45.950	2.240
High resolution limit [Å]	2.180	9.750	2.180
Rmerge	0.154	0.039	2.273
Rmeas	0.168	0.042	2.461
Total number of observations	315277
Number of reflections	49587	646	3608
<I/σ(I)>	9.98	31.38	1.3
Completeness [%]	99.8	98.3	99.7
Redundancy	6.358	5.604	6.772
CC(1/2)	0.996	0.998	0.458

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