3NU0
Design, Synthesis, Biological Evaluation and X-ray Crystal Structure 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 |
Wavelength(s) | 0.975 |
Spacegroup name | H 3 |
Unit cell lengths | 84.395, 84.395, 78.193 |
Unit cell angles | 90.00, 90.00, 120.00 |
Refinement procedure
Resolution | 33.100 - 1.350 |
R-factor | 0.18149 |
Rwork | 0.180 |
R-free | 0.20927 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | u072 |
RMSD bond length | 0.035 |
RMSD bond angle | 2.992 |
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] | 33.100 | 1.420 |
High resolution limit [Å] | 1.350 | 1.350 |
Rmerge | 0.063 | 0.390 |
Number of reflections | 45587 | |
<I/σ(I)> | 27 | 8.6 |
Completeness [%] | 100.0 | 100 |
Redundancy | 12.5 | 12.1 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 6.9 | 293 | 100 mM KPO4, 69% saturated AmSO4, 3% v/v ethanol, pH 6.9, VAPOR DIFFUSION, HANGING DROP, temperature 200K, temperature 293K |