4QGE

phosphodiesterase-9A in complex with inhibitor WYQ-C36D

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
Detector	ADSC QUANTUM 315
Wavelength(s)	1.05
Spacegroup name	P 41 21 2
Unit cell lengths	103.580, 103.580, 268.657
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	30.000 - 2.000
Rwork	0.241
R-free	0.26800
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	PDE9 catalytic domain
RMSD bond length	0.006
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
Low resolution limit [Å]	30.000
High resolution limit [Å]	2.000
Rmerge	0.065
Number of reflections	91112
<I/σ(I)>	23
Completeness [%]	91.5
Redundancy	10.5

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.5	277	The crystals of PDE9A2 were grown by using hanging drop vapor diffusion method. The PDE9A2 (181 506) (8-10 mg/mL) in a buffer of 50 mM NaCl, 20 mM Tris HCl, pH 7.5, 1 mM -mercaptoethanol, and 1 mM EDTA was mixed with 2 mM IBMX overnight before setting-up of crystallization against the well buffer of 0.1 M HEPES (pH 7.5), 3.0 M sodium formate at 4 C. Crystals of the PDE9-3r complex were prepared by soaking PDE9-IBMX cocrystals in the crystallization buffer plus 2 mM 3r at 25oC for 3 days., VAPOR DIFFUSION, HANGING DROP, temperature 277K