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 |