4LI8

TANKYRASE-1 complexed with small molecule inhibitor 2-[4-(4-fluorobenzoyl)piperidin-1-yl]-N-[(4-oxo-3,5,7,8-tetrahydro-4H-pyrano[4,3-d]pyrimidin-2-yl)methyl]-N-(thiophen-2-ylmethyl)acetamide

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SLS BEAMLINE X06SA
Synchrotron site	SLS
Beamline	X06SA
Temperature [K]	100
Detector technology	PIXEL
Collection date	2009-02-01
Detector	PSI PILATUS 6M
Wavelength(s)	1
Spacegroup name	C 1 2 1
Unit cell lengths	124.700, 43.100, 88.100
Unit cell angles	90.00, 91.30, 90.00

Refinement procedure

Resolution	44.039 - 2.521
R-factor	0.2105
Rwork	0.207
R-free	0.28270
Structure solution method	FOURIER METHODS
RMSD bond length	0.005
RMSD bond angle	0.939
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHENIX
Refinement software	PHENIX ((phenix.refine))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.670
High resolution limit [Å]	2.521	2.521
Rmerge	0.105	0.353
Number of reflections	15321
<I/σ(I)>	9.41	3.57
Completeness [%]	98.2	98.7
Redundancy	3.17	3.25

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	5.8	298	EQUAL VOLUMES (2 UL) OF RESERVIOR SOLUTION AND PROTEIN SOLUTION WERE MIXED AND SET AS HANGING DROPS. 15% PEG3350, 100MM BIS-TRIS PH5.8, 310MM AMMONIUM SULFATE. PROTEIN SOLUTION: 20 MG/ML IN 25 MM TRIS PH8, 200MM NACL, 1MM TCEP, 1MM PJ34. CRYSTALS WERE THEN MOVED INTO A SOAKING SOLUTION CONTAINING 18% PEG 3350, 320MM AMMONIUM SULFATE, 100MM BIS- TRIS PH 5.8, 0.2 MM inhibitor. , VAPOR DIFFUSION, HANGING DROP, temperature 298K