6Y2U

Crystal structure of the cAMP-dependent protein kinase A cocrystallized with aminofasudil and PKI (5-24)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID29
Synchrotron site	ESRF
Beamline	ID29
Temperature [K]	100
Detector technology	PIXEL
Collection date	2017-02-17
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.97900
Spacegroup name	P 21 21 21
Unit cell lengths	58.706, 71.119, 107.976
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.270 - 1.930
R-factor	0.1866
Rwork	0.185
R-free	0.22150
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	6f14
RMSD bond length	0.007
RMSD bond angle	0.777
Data reduction software	XDS
Data scaling software	XDS
Phasing software	PHASER
Refinement software	PHENIX (1.15.2_3472)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	45.274	2.040
High resolution limit [Å]	1.927	1.930
Number of reflections	34803	5493
<I/σ(I)>	10.89	2.81
Completeness [%]	99.8
Redundancy	7.4

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.9	277	100 mM MES-BIS-Tris-Buffer, 1 mM dithiothreitol, 0.1 mM sodium EDTA, 75 mM LiCl, 0.2 Mega8, 5 mM aminofasudil (in DMSO), 0.5 mM PKI (5-24) and 18-23 % methanol (v/v)0.004 mL drop volume, 0.5 mL reservoir volume