6YQJ

Crystal structure of cAMP-dependent Protein Kinase (PKA) in complex with open-chain Fasudil-derivative 2-[isoquinolin-5-ylsulfonyl(propyl)amino]ethylazanium (soaked)

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	2013-12-14
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.918409
Spacegroup name	P 21 21 21
Unit cell lengths	58.272, 72.662, 109.372
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	36.330 - 1.580
R-factor	0.16
Rwork	0.158
R-free	0.20050
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1q8w
RMSD bond length	0.008
RMSD bond angle	0.964
Data reduction software	XDS
Data scaling software	XDS
Phasing software	PHASER
Refinement software	PHENIX (1.17.1_3660)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	45.459	1.670
High resolution limit [Å]	1.576	1.580
Number of reflections	62707	8401
<I/σ(I)>	15.67	2.39
Completeness [%]	96.6
Redundancy	5.2

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.9	277	0.24mM PKA, 30mM MBT (MES/Bis-Tris Buffer pH 6.2-6.9), 1mM DTT, 0.1mM EDTA, 75mM LiCl, 0.3mM Mega 8, 0.7mM PKI, 16%(v/v) methanol; soaking in buffer described with 0.12mM ligand solved in DMSO and 30%(v/v) MPD