1GI1

A NOVEL SERINE PROTEASE INHIBITION MOTIF INVOLVING A MULTI-CENTERED SHORT HYDROGEN BONDING NETWORK AT THE ACTIVE SITE

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU RU200
Temperature [K]	298
Detector technology	IMAGE PLATE
Collection date	2000-01-29
Detector	RIGAKU RAXIS IV
Spacegroup name	P 21 21 21
Unit cell lengths	54.920, 58.830, 67.370
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	7.000 - 1.420
R-factor	0.166
Rwork	0.167
R-free	0.18600
Structure solution method	FOURIER SYNTHESIS
RMSD bond length	0.018
RMSD bond angle	3.800 *
Data reduction software	bioteX
Data scaling software	bioteX
Refinement software	X-PLOR (3.851)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	34.480	1.480
High resolution limit [Å]	1.320	1.420
Rmerge	0.071	0.250
Total number of observations	72876 *
Number of reflections	31541
<I/σ(I)>	10.1
Completeness [%]	61.2	35.7
Redundancy	2.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	Vapor diffusion, hanging drop *	8.1	298	magnesium sulfate soak at target pH (6.4). vapor diffusion at 298 K, pH 8.10

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	drop	protein	10 (mg/ml)
2	1	reservoir	HEPES	0.10 (M)	pH7.5 or 8.2
3	1	reservoir		0.30 (M)
4	1	reservoir	PEG5000 MME	22 (%(v/v))