9FDN

Human phosphoglycerate kinase in complex with ATP and 3PG formed by cross-soaking a TSA crystal

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	DIAMOND BEAMLINE I03
Synchrotron site	Diamond
Beamline	I03
Temperature [K]	83
Detector technology	PIXEL
Collection date	2016-07-15
Detector	DECTRIS EIGER2 XE 16M
Wavelength(s)	0.9763
Spacegroup name	P 21 21 21
Unit cell lengths	39.040, 91.100, 108.200
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	54.100 - 1.580
R-factor	0.1795
Rwork	0.178
R-free	0.20450
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.010
RMSD bond angle	1.242
Data reduction software	DIALS
Data scaling software	xia2
Phasing software	PHENIX
Refinement software	PHENIX ((1.18.2_3874: ???))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	54.100	1.640
High resolution limit [Å]	1.580	1.580
Rmerge	0.033	0.635
Rmeas	0.047	0.898
Rpim	0.033	0.635
Number of reflections	53778	5282
<I/σ(I)>	12	1.4
Completeness [%]	99.9	99.9
Redundancy	2
CC(1/2)	0.999	0.483

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6.5	298	MgF3 TSA complex crystals were formed from 50 mM Tris (pH 7.5), 20 mM DTT, 25 mM MgCl2, 50 mM 3PG, and 10 mM ADP supplemented with 20 mM NH4F and 1 mM deferoxamine, in 28-33% PEG 2000 MME and 0.1 M Bis/Tris pH 6.5. These were cross-soaked in 35% PEG 2000 MME; 0.1 M Bis/Tris pH 6.5, 20 mM DTT, 2.5mM EDTA, 10mM ATP and 50 mM 3PG