6P5P
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 5.0.2 |
Synchrotron site | ALS |
Beamline | 5.0.2 |
Temperature [K] | 100 |
Detector technology | CCD |
Collection date | 2011-11-23 |
Detector | ADSC QUANTUM 315r |
Wavelength(s) | 0.97648 |
Spacegroup name | P 1 21 1 |
Unit cell lengths | 89.171, 146.438, 111.300 |
Unit cell angles | 90.00, 97.13, 90.00 |
Refinement procedure
Resolution | 25.000 - 3.300 |
R-factor | 0.2073 |
Rwork | 0.206 |
R-free | 0.23570 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 2f2u |
RMSD bond length | 0.007 |
RMSD bond angle | 1.327 |
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 | 3.360 |
High resolution limit [Å] | 3.300 | 8.940 | 3.300 |
Rmerge | 0.147 | 0.033 | 0.890 |
Total number of observations | 180093 | ||
Number of reflections | 42899 | 2207 | 2082 |
<I/σ(I)> | 5.9 | ||
Completeness [%] | 99.9 | 100 | 99.6 |
Redundancy | 4.2 | 4.2 | 4.1 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, SITTING DROP | 5.2 | 293 | 0.8 M trisodium citrate, 0.1 M citrate, pH 5.2, Silver Bullets Bio B12 (0.025% thymidine-5'-triphosphate sodium salt, 0.025% alpha-ketoglutaric acid disodium salt, 0.025% 2-nitrophenyl beta-D-galactopyranoside, 0.025% cis-aconitic acid, 0.002 M HEPES sodium, pH 6.8) |