7G5F

Crystal Structure of rat Autotaxin in complex with 1H-benzotriazol-5-yl-[rac-(1R,2R,6S,7S)-9-[4-(cyclopropylmethoxy)naphthalene-2-carbonyl]-4,9-diazatricyclo[5.3.0.02,6]decan-4-yl]methanone, i.e. SMILES N1(C[C@H]2[C@@H](C1)[C@H]1[C@@H]2CN(C1)C(=O)c1ccc2c(c1)N=NN2)C(=O)c1cc(c2c(c1)cccc2)OCC1CC1 with IC50=0.00985223 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	2012-10-28
Detector	PSI PILATUS 6M
Wavelength(s)	0.99986
Spacegroup name	P 21 21 21
Unit cell lengths	84.078, 91.953, 120.100
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.980 - 2.300
R-factor	0.2182
Rwork	0.215
R-free	0.26990
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	inhouse model
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	PHENIX (1.20.1_4487)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	45.980	45.980	2.360
High resolution limit [Å]	2.300	10.290	2.300
Rmerge	0.195	0.048	1.625
Rmeas	0.215	0.053	1.788
Total number of observations	247830
Number of reflections	41902	550	3055
<I/σ(I)>	7.14	20.03	1.38
Completeness [%]	99.4	98.4	99.3
Redundancy	5.915	5.947	5.792
CC(1/2)	0.992	0.998	0.730

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