3GHC
Design, Synthesis, and X-ray Crystal Structure of Classical and Nonclassical 2-amino-4-oxo-5-substituted-6-thieno[2,3-d]pyrimidines as dual thymidylate synthase and dihydrofolate reductase inhibitors and as potential antitumor agenst
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | SSRL BEAMLINE BL11-1 |
| Synchrotron site | SSRL |
| Beamline | BL11-1 |
| Temperature [K] | 200 |
| Detector technology | CCD |
| Collection date | 2008-06-13 |
| Detector | MARMOSAIC 325 mm CCD |
| Wavelength(s) | 0.9422 |
| Spacegroup name | H 3 |
| Unit cell lengths | 84.356, 84.356, 77.767 |
| Unit cell angles | 90.00, 90.00, 120.00 |
Refinement procedure
| Resolution | 22.510 - 1.300 |
| R-factor | 0.17143 |
| Rwork | 0.170 |
| R-free | 0.19850 |
| Structure solution method | MOLECULAR REPLACEMENT |
| Starting model (for MR) | 1u72 |
| RMSD bond length | 0.032 |
| RMSD bond angle | 2.580 |
| Data reduction software | MOSFLM |
| Data scaling software | SCALA |
| Phasing software | MOLREP |
| Refinement software | REFMAC (5.5.0088) |
Data quality characteristics
| Overall | Outer shell | |
| Low resolution limit [Å] | 53.220 | 1.370 |
| High resolution limit [Å] | 1.300 | 1.300 |
| Rmerge | 0.045 | 0.143 |
| Number of reflections | 48164 | |
| <I/σ(I)> | 10.3 | |
| Completeness [%] | 99.8 | 99.3 |
| Redundancy | 5.3 | 4.3 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, HANGING DROP | 6.9 | 298 | 100 mN KPO4, pH 6.9, 30% sat. AmSO4, 3% v/v ethanol, VAPOR DIFFUSION, HANGING DROP, temperature 298K |
