5M6V
Cocrystal structure of cAMP-dependent Protein Kinase (PKA) in complex with a double methylated Fasudil-derivative
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | ESRF BEAMLINE BM14 |
Synchrotron site | ESRF |
Beamline | BM14 |
Temperature [K] | 100 |
Detector technology | CCD |
Collection date | 2015-04-13 |
Detector | MARMOSAIC 225 mm CCD |
Wavelength(s) | 0.97625 |
Spacegroup name | P 21 21 21 |
Unit cell lengths | 58.537, 73.183, 108.847 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 31.028 - 1.418 |
R-factor | 0.145 |
Rwork | 0.143 |
R-free | 0.17400 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 1q8w |
RMSD bond length | 0.008 |
RMSD bond angle | 1.034 |
Data reduction software | XDS |
Data scaling software | XDS |
Phasing software | PHASER |
Refinement software | PHENIX ((1.10.1_2155: ???)) |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 45.713 | 1.500 |
High resolution limit [Å] | 1.418 | 1.420 |
Rmerge | 0.476 | |
Number of reflections | 88220 | |
<I/σ(I)> | 23.58 | 3.86 |
Completeness [%] | 98.9 | 97.1 |
Redundancy | 7.284 | 7.287 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 6.9 | 277.15 | Drop: 10 mg/ml PKA (0.240 mM) 30 mM MBT (MES/Bis-Tris Puffer pH 6.9) 1 mM DTT 0.1 mM EDTA 75 mM LiCl 0.03 mM Mega 8 0.07mM PKI (Sigma: P7739) 1.2 mM ligand solved in DMSO (50 mM Stock) Reservoir: 18% Methanol 0.003 mL drop volume, 0.4 mL reservoir volume |