1PD2

CRYSTAL STRUCTURE OF HEMATOPOIETIC PROSTAGLANDIN D SYNTHASE COMPLEX WITH GLUTATHIONE

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	PHOTON FACTORY BEAMLINE BL-6A
Synchrotron site	Photon Factory
Beamline	BL-6A
Temperature [K]	298
Detector technology	IMAGE PLATE
Detector	RIGAKU
Spacegroup name	P 31 2 1
Unit cell lengths	56.500, 56.500, 233.400
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	6.000 - 2.300
R-factor	0.204 *
Rwork	0.204
R-free	0.28900
Structure solution method	MIRAS
RMSD bond length	0.010
RMSD bond angle	1.613
Data reduction software	ROTAVATA
Data scaling software	WEIS
Phasing software	PHASES
Refinement software	X-PLOR (3.1)

Data quality characteristics

	Overall
Low resolution limit [Å]	40.000
High resolution limit [Å]	2.300
Rmerge	0.085
Number of reflections	77899
Completeness [%]	95.1
Redundancy	4

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	Vapor diffusion, hanging drop *	7.5 *	22.5 *	VAPOR DIFFUSION METHOD RESERVOIR SOLUTION: 18% (W/V) PEG 6K, 100 MM AMMONIUM CITRATE 5MM CACL2, 10MM DTT, 2% (V/V) 1,4-DIOXANE PROTEIN SOLUTION: 7.3 MG/ML PROTEIN (50 MM TRIS-HCL [PH 7.5]) EACH 4 UL WAS MIXED FOR DROPLET

Crystallization Reagents

ID	crystal ID	solution ID	reagent name	concentration	details
1	1	1	7.3 MG/ML PROTEIN (50 MM TRIS-HCL [PH 7.5})
2	1	2	10% (W/V) PEG 6K
3	1	2	100 MM AMMONIUM CITRATE
4	1	2	5MM CACL2
5	1	2	10MM DTT
6	1	2	2% (V/V) 1,4-DIOXANE

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	drop	protein	7.3 (mg/ml)
2	1	drop	Tris-HCl	50 (mM)
3	1	drop	GSH	10 (mM)
4	1	reservoir	PEG6000	18 (%(w/v))
5	1	reservoir	ammonium citrate	100 (mM)
6	1	reservoir		5 (mM)
7	1	reservoir	dithiothreitol	10 (mM)
8	1	reservoir	1,4-dioxane	2 (%(v/v))