1S2A

Crystal structures of prostaglandin D2 11-ketoreductase in complex with the non-steroidal anti-inflammatory drugs flufenamic acid and indomethacin

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID14-2
Synchrotron site	ESRF
Beamline	ID14-2
Temperature [K]	100
Detector technology	CCD
Collection date	2002-02-09
Detector	ADSC QUANTUM 4
Wavelength(s)	0.93
Spacegroup name	P 21 21 21
Unit cell lengths	55.808, 63.074, 96.200
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	20.000 - 1.700
R-factor	0.17356
Rwork	0.172
R-free	0.19800 *
Structure solution method	isomorphous replacement
Starting model (for MR)	1s1p
RMSD bond length	0.009
RMSD bond angle	1.600 *
Data reduction software	MOSFLM
Data scaling software	CCP4 ((SCALA))
Phasing software	CNS
Refinement software	REFMAC (5.1.19)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	20.000 *	1.790
High resolution limit [Å]	1.700	1.700
Rmerge	0.049 *	0.200 *
Total number of observations	127566 *
Number of reflections	37296	4785 *
<I/σ(I)>	18.7	4.7
Completeness [%]	98.0	88.3
Redundancy	3.4	2.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7 *	291	PEG, pH 4.6, VAPOR DIFFUSION, HANGING DROP, temperature 291K

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	drop	protein	6 (mg/ml)
2	1	drop	potassium phosphate	10 (mM)	pH7.0
3	1	drop	dithiothreitol	1 (mM)
4	1	drop	EDTA	1 (mM)
5	1	drop	NADP+	2 (mM)
6	1	reservoir	PEG4000	25 (%(w/v))
7	1	reservoir	sodium citrate	100 (mM)	pH6.0
8	1	reservoir	MPD	2.5 (%(v/v))
9	1	reservoir	ammonium acetate	800 (mM)