1JWH
Crystal Structure of Human Protein Kinase CK2 Holoenzyme
Experimental procedure
| Experimental method | SINGLE WAVELENGTH |
| Source type | SYNCHROTRON |
| Source details | EMBL/DESY, HAMBURG BEAMLINE BW7B |
| Synchrotron site | EMBL/DESY, HAMBURG |
| Beamline | BW7B |
| Temperature [K] | 100 |
| Detector technology | IMAGE PLATE |
| Collection date | 2000-01-26 |
| Detector | MARRESEARCH |
| Wavelength(s) | 0.8428 |
| Spacegroup name | P 63 |
| Unit cell lengths | 175.990, 175.990, 93.666 |
| Unit cell angles | 90.00, 90.00, 120.00 |
Refinement procedure
| Resolution | 60.000 * - 3.100 |
| R-factor | 0.267 * |
| Rwork | 0.267 |
| R-free | 0.33800 |
| Structure solution method | MOLECULAR REPLACEMENT |
| Starting model (for MR) | POLY-ALANINE BACKBONE OF CK2A FROM ZEA MAYS (PDB ENTRY 1DAW) |
| RMSD bond length | 0.009 |
| RMSD bond angle | 22.200 * |
| Data reduction software | DENZO |
| Data scaling software | SCALEPACK |
| Phasing software | AMoRE |
| Refinement software | CNS (1.0) |
Data quality characteristics
| Overall | Outer shell | |
| Low resolution limit [Å] | 59.300 | 3.200 |
| High resolution limit [Å] | 3.100 | 3.100 |
| Rmerge | 0.096 * | 0.420 * |
| Total number of observations | 268848 * | |
| Number of reflections | 29935 | |
| <I/σ(I)> | 16.7 | 2.6 |
| Completeness [%] | 98.4 | 90.4 |
| Redundancy | 8.8 | 6 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, SITTING DROP | 8.5 * | 12 * | initial composition of the drop: 3 ul rhCK2 stock solution [5 mg/ml enzyme in 25 mM Tris/HCl, 300 mM NaCl, 1 mM dithiothreitole, pH 8.5], 1.5 ul reservoir solution [20 % (w/v) PEG3350, 200 mM dipotassium hydrogenphosphate], 3 ul 1 mM adenylyl imidodiphosphate (AMPPNP), 3 ul 2 mM magnesium chloride, 2 ul 10 % (w/v) polyethylene glycol 400 dodecylether (Thesit), pH 9.3, VAPOR DIFFUSION, SITTING DROP, temperature 285K |
Crystallization Reagents in Literatures
| ID | crystal ID | solution | reagent name | concentration (unit) | details |
| 1 | 1 | drop | protein | 5.0 (mg/ml) | |
| 2 | 1 | drop | Tris-HCl | 25 (mM) | |
| 3 | 1 | drop | 300 (mM) | ||
| 4 | 1 | drop | dithiothreitol | 1 (mM) | pH8.5 |
| 5 | 1 | drop | 2.0 (mM) | ||
| 6 | 1 | drop | AMPPNP | 1 (mM) | |
| 7 | 1 | drop | PEG400 | 10 (%(w/v)) | dodecylether |
| 8 | 1 | reservoir | PEG3350 | 20 (%(w/v)) | |
| 9 | 1 | reservoir | potassium phosphate | 200 (mM) | pH9.3 |
