5M0B
Cocrystal structure of cAMP-dependent Protein Kinase (PKA) in complex with a short-chained N-(2-aminoethyl)isoquinoline-5-sulfonamide) Fasudil-derivative (Ligand 03)
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 | 57.945, 71.736, 109.922 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 39.876 - 1.506 |
R-factor | 0.1334 |
Rwork | 0.132 |
R-free | 0.15940 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 1q8w |
RMSD bond length | 0.008 |
RMSD bond angle | 0.955 |
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] | 45.080 | 1.600 |
High resolution limit [Å] | 1.506 | 1.506 |
Rmerge | 0.498 | |
Number of reflections | 73047 | |
<I/σ(I)> | 26.28 | 3.89 |
Completeness [%] | 99.9 | 99.7 |
Redundancy | 7.32 | 7.26 |
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 |