4LI6

TANKYRASE-1 Complexed with small molecule inhibitor N-[(4-oxo-3,4-dihydroquinazolin-2-yl)methyl]-3-phenyl-N-(thiophen-2-ylmethyl)propanamide

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU FR-E SUPERBRIGHT
Temperature [K]	100
Detector technology	CCD
Collection date	2008-09-24
Detector	RIGAKU SATURN 92
Wavelength(s)	1.54178
Spacegroup name	C 1 2 1
Unit cell lengths	124.082, 44.814, 87.846
Unit cell angles	90.00, 90.22, 90.00

Refinement procedure

Resolution	26.520 - 2.050
R-factor	0.1758
Rwork	0.172
R-free	0.22390
Structure solution method	FOURIER METHODS
RMSD bond length	0.007
RMSD bond angle	1.073
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	PHENIX
Refinement software	PHENIX ((phenix.refine: 1.8_1069))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.120
High resolution limit [Å]	2.050	2.050
Rmerge	0.116	0.379
Number of reflections	30133
<I/σ(I)>		4.91
Completeness [%]	98.0	96.1
Redundancy		3.4

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