6P5M

Discovery of a Novel, Highly Potent, and Selective Thieno[3,2-d]pyrimidinone-Based Cdc7 inhibitor with a Quinuclidine Moiety (TAK-931) as an Orally Active Investigational Anti-Tumor Agent

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ALS BEAMLINE 5.0.3
Synchrotron site	ALS
Beamline	5.0.3
Temperature [K]	100
Detector technology	CCD
Collection date	2011-03-03
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.97648
Spacegroup name	P 1 21 1
Unit cell lengths	89.456, 146.416, 111.876
Unit cell angles	90.00, 97.12, 90.00

Refinement procedure

Resolution	25.000 - 2.650
R-factor	0.195
Rwork	0.193
R-free	0.22500
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2f2u
RMSD bond length	0.007
RMSD bond angle	1.328
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	PHASER
Refinement software	REFMAC (5.8.0238)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	2.700
High resolution limit [Å]	2.650	7.190	2.650
Rmerge	0.103	0.037	0.788
Total number of observations	346085
Number of reflections	83024	4257	4094
<I/σ(I)>	9.1
Completeness [%]	99.9	100	99.3
Redundancy	4.2	4.1	3.9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	5.1	293	0.8 M trisodium citrate, 0.1 M citrate, pH 5.1