3NTZ
Design, Synthesis, Biological Evaluation and X-ray Crystal Structures of Novel Classical 6,5,6-tricyclicbenzo[4,5]thieno[2,3-d]pyrimidines as Dual Thymidylate Synthase and Dihydrofolate Reductase Inhibitors
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | SSRL BEAMLINE BL9-2 |
| Synchrotron site | SSRL |
| Beamline | BL9-2 |
| Temperature [K] | 200 |
| Detector technology | CCD |
| Collection date | 2008-12-06 |
| Detector | MARMOSAIC 325 mm CCD |
| Spacegroup name | H 3 |
| Unit cell lengths | 84.287, 84.287, 77.792 |
| Unit cell angles | 90.00, 90.00, 120.00 |
Refinement procedure
| Resolution | 26.610 - 1.350 |
| R-factor | 0.187 |
| Rwork | 0.186 |
| R-free | 0.20300 |
| Structure solution method | MOLECULAR REPLACEMENT |
| Starting model (for MR) | U072 |
| RMSD bond length | 0.031 |
| RMSD bond angle | 2.844 |
| 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 | 1.420 |
| High resolution limit [Å] | 1.350 | 1.350 |
| Rmerge | 0.053 | 0.610 |
| Number of reflections | 45260 | |
| <I/σ(I)> | 15.3 | 1.6 |
| Completeness [%] | 100.0 | 100 |
| Redundancy | 3.7 | 3.7 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | 6.9 | 293 | 100 mM KPO4, 66% saturated AmSO4, 3% v/v ethanol, pH 6.9, VAPOR DIFFUSION, HANGING DROP, temperature 200K, temperature 293K |
