8PPC

Human inositol 1,4,5-trisphosphate 3-kinase A (IP3K) catalytic domain in complex with L-chiro-inositol 2,3,5-trisphosphate/ATP/Mn

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ALBA BEAMLINE XALOC
Synchrotron site	ALBA
Beamline	XALOC
Temperature [K]	100
Detector technology	PIXEL
Collection date	2021-06-19
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.979264
Spacegroup name	C 2 2 21
Unit cell lengths	71.915, 97.904, 191.881
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	49.660 - 1.920
R-factor	0.19451
Rwork	0.193
R-free	0.21886
Structure solution method	FOURIER SYNTHESIS
RMSD bond length	0.008
RMSD bond angle	1.500
Data reduction software	XDS
Data scaling software	XDS
Phasing software	REFMAC
Refinement software	REFMAC (v5.8.0258)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	49.660	1.970
High resolution limit [Å]	1.920	1.920
Rpim	0.032	0.299
Number of reflections	51230	2906
<I/σ(I)>	13.3	1.8
Completeness [%]	98.4	84.8
Redundancy	10	7.6
CC(1/2)	0.997	0.799

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	8.5	291	0.80 M sodium citrate, 0.1M Tris pH 8.5 and 0.1 M NaCl. Protein:precipitant ratio 1:1. Protein concentration: 9 mg/ml. Protein buffer: 20 mM Tris pH 7.5, 50 mM ammonium sulfate and 2 mM DTT. Soaking 2h with 1.5 M lithium sulfate, 0.1 M Tris pH 8.5, 5 mM ligand, 3 mM ATP and 3 mM MnCl2.