6YNA

Crystal structure of cAMP-dependent Protein Kinase (PKA) in complex with Fasudil (M77, 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	2015-02-07
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.918409
Spacegroup name	P 21 21 21
Unit cell lengths	58.313, 72.547, 109.039
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	30.850 - 1.470
R-factor	0.1646
Rwork	0.163
R-free	0.18900
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1q8w
RMSD bond length	0.005
RMSD bond angle	0.775
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]	45.450	1.560
High resolution limit [Å]	1.468	1.470
Number of reflections	79455	12522
<I/σ(I)>	27.59	3.79
Completeness [%]	99.7
Redundancy	6.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.9	277	0.24mM PKA, 30mM 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