4MD6

Crystal structure of PDE5 in complex with inhibitor 5R

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	NSLS BEAMLINE X29A
Synchrotron site	NSLS
Beamline	X29A
Temperature [K]	100
Detector technology	CCD
Collection date	2013-06-20
Detector	ADSC QUANTUM 315
Wavelength(s)	1
Spacegroup name	P 31 2 1
Unit cell lengths	74.106, 74.106, 132.344
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	30.000 - 2.000
R-factor	0.217
Rwork	0.217
R-free	0.24750
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.005
RMSD bond angle	1.100
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	AMoRE
Refinement software	CNS

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	30.000
High resolution limit [Å]	2.000	2.000
Rmerge	0.065
Number of reflections	29180
<I/σ(I)>	14
Completeness [%]	100.0
Redundancy	22.8

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.5	277	6-10 mg/mL unliganded PDE5A1 in storage buffer (50 mM sodium chloride, 20 mM Tris-HCl, pH 7.5, 1 mM BME, 1 mM EDTA) against 0.2 M magnesium sulfate, 0.1 M sodium cacodylate, pH 6.5, 18% PEG3350, VAPOR DIFFUSION, HANGING DROP, temperature 277K