3BE9
Structure-based design and synthesis of novel macrocyclic pyrazolo[1,5-a] [1,3,5]triazine compounds as potent inhibitors of protein kinase CK2 and their anticancer activities
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | ROTATING ANODE |
| Source details | ENRAF-NONIUS FR591 |
| Temperature [K] | 112 |
| Detector technology | IMAGE PLATE |
| Collection date | 2005-12-21 |
| Detector | MAR scanner 345 mm plate |
| Spacegroup name | C 1 2 1 |
| Unit cell lengths | 143.327, 59.578, 44.835 |
| Unit cell angles | 90.00, 103.42, 90.00 |
Refinement procedure
| Resolution | 32.700 - 2.000 |
| Rwork | 0.190 |
| R-free | 0.22800 |
| Structure solution method | FOURIER SYNTHESIS |
| Starting model (for MR) | 2pvj |
| RMSD bond length | 0.005 |
| RMSD bond angle | 1.910 |
| Data reduction software | DENZO |
| Data scaling software | SCALEPACK |
| Phasing software | CNX |
| Refinement software | CNX |
Data quality characteristics
| Overall | Outer shell | |
| Low resolution limit [Å] | 32.700 | 2.070 |
| High resolution limit [Å] | 2.000 | 2.000 |
| Rmerge | 0.084 | 0.409 |
| Number of reflections | 23749 | |
| <I/σ(I)> | 16.4 | 2.5 |
| Completeness [%] | 95.0 | 92 |
| Redundancy | 3.54 | 3.3 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, HANGING DROP | 8 | 297 | 14% PEG 4000, 0.05M Sodium Acetate, 0.10M TRISHCL, pH 8.0, VAPOR DIFFUSION, HANGING DROP, temperature 297K |
