3BJC

Crystal structure of the PDE5A catalytic domain in complex with a novel inhibitor

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	2006-09-05
Detector	ADSC QUANTUM 315
Wavelength(s)	1.1
Spacegroup name	P 31 2 1
Unit cell lengths	73.755, 73.755, 132.509
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	30.000 - 2.000
Rwork	0.197
R-free	0.22100
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	PDE5 catalytic domain in complex with IBMX
RMSD bond length	0.005
RMSD bond angle	1.200
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	2.100
High resolution limit [Å]	2.000	2.000
Rmerge	0.073	0.350
Number of reflections	26266
<I/σ(I)>	11	2
Completeness [%]	91.1	49.8
Redundancy	9.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.5	298	The PDE5A1-12 complex was prepared by mixing 1 mM compound 12 with 15 mg/mL PDE5A1 that was stored in a buffer of 20 mM Tris.base, pH 7.5, 50 mM NaCl, 1 mM beta-mercaptoethanol, and 1 mM EDTA. The protein drop was prepared by mixing protein with well buffer and crystallized against a well buffer of 2.0 M sodium formate, 0.1 M sodium citrate, pH 5.6, 5% ethanol at 298K, VAPOR DIFFUSION, HANGING DROP