5DGH

Crystal structure of the catalytic domain of human diphosphoinositol pentakisphosphate kinase 2 (PPIP5K2) in complex with AMP-PNP and 5-(PCP)-IP5

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	2015-06-12
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	1.0
Spacegroup name	P 21 21 21
Unit cell lengths	87.900, 110.340, 41.253
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	29.040 - 2.100
R-factor	0.18945
Rwork	0.187
R-free	0.23140
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	3t7a
RMSD bond length	0.009
RMSD bond angle	1.450
Data scaling software	HKL-2000
Refinement software	REFMAC (5.7.0032)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.350
High resolution limit [Å]	2.100	2.100
Rmerge		0.382
Number of reflections	23365
<I/σ(I)>	16.5	2.5
Completeness [%]	96.8	87.2
Redundancy	4.8	3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7	277	12% (w/v) PEG 3350, 20 mM MgCl2, 0.1 M HEPES, pH 7.0, 1 mM AMP-PNP and 2 mM CdCl2. The crystals were transferred to a stabilizing buffer containing 22% (w/v) PEG 3350, 10 mM MgCl2, 0.1 M sodium acetate, pH 5.2 at 4 oC overnight. The crystals were soaked under the above stabilizing buffer for three days with 2 mM compound.