4Y87

Crystal structure of phosphodiesterase 9 in complex with (R)-C33 (6-{[(1R)-1-(4-chlorophenyl)ethyl]amino}-1-cyclopentyl-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-4-one)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 22-BM
Synchrotron site	APS
Beamline	22-BM
Temperature [K]	100
Detector technology	CCD
Collection date	2014-12-13
Detector	ADSC QUANTUM 315
Wavelength(s)	1.05
Spacegroup name	P 41 21 2
Unit cell lengths	105.436, 105.436, 270.056
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	98.220 - 3.100
R-factor	0.20719
Rwork	0.205
R-free	0.24742
RMSD bond length	0.007
RMSD bond angle	1.085
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	PHASER
Refinement software	REFMAC (5.8.0073)

Data quality characteristics

	Overall
Low resolution limit [Å]	98.220
High resolution limit [Å]	3.100
Number of reflections	24552
<I/σ(I)>	7.6
Completeness [%]	84.9
Redundancy	6.6

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.5	277	The PDE9A2 (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 C33 or (R)-C33 and crystallized against a well buffer of 1.8 - 2.0 M sodium formate.