9FDF

Human phosphoglycerate kinase in with mixture of products and substrates produced by cross-soaking a TSA crystal

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	DIAMOND BEAMLINE I04-1
Synchrotron site	Diamond
Beamline	I04-1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2012-07-23
Detector	DECTRIS EIGER2 XE 9M
Wavelength(s)	0.933
Spacegroup name	P 21 21 21
Unit cell lengths	39.430, 92.010, 108.610
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	37.060 - 1.440
R-factor	0.1423
Rwork	0.141
R-free	0.16620
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.004
RMSD bond angle	0.880
Data reduction software	xia2
Data scaling software	xia2
Phasing software	PHENIX
Refinement software	PHENIX (1.21.1_5286)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	37.060	1.490
High resolution limit [Å]	1.440	1.440
Rmerge	0.030	0.353
Rmeas	0.042	0.499
Rpim	0.030	0.353
Number of reflections	71262	6991
<I/σ(I)>	14.2	2.4
Completeness [%]	98.5	97.8
Redundancy	1.9	1.9
CC(1/2)	0.999	0.737

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6.5	298	crystals were initially produced 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 then cross-soaked with 35% PEG 2000 MME; 0.1 M Bis/Tris pH 6.5, 20 mM DTT, and 50 mM 3PG and 0.1mM deferoxamine