5M0L
Cocrystal structure of cAMP-dependent Protein Kinase (PKA) in complex with the methylated Fasudil-derived fragment N-methylisoquinoline-5-sulfonamide (Ligand 02)
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | BESSY BEAMLINE 14.1 |
Synchrotron site | BESSY |
Beamline | 14.1 |
Temperature [K] | 100 |
Detector technology | PIXEL |
Collection date | 2014-11-22 |
Detector | DECTRIS PILATUS3 6M |
Wavelength(s) | 0.91841 |
Spacegroup name | P 21 21 21 |
Unit cell lengths | 65.814, 79.707, 84.511 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 32.907 - 1.465 |
R-factor | 0.1535 |
Rwork | 0.152 |
R-free | 0.17280 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 1q8w |
RMSD bond length | 0.008 |
RMSD bond angle | 1.046 |
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] | 34.090 | 1.550 |
High resolution limit [Å] | 1.465 | 1.465 |
Rmerge | 0.495 | |
Number of reflections | 75918 | |
<I/σ(I)> | 19.11 | 2.7 |
Completeness [%] | 98.7 | 97.4 |
Redundancy | 4.07 | 4.18 |
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 (100 mM Stock) Reservoir: 16% Methanol 0.003 mL drop volume, 0.4 mL reservoir volume |