1O2G

Elaborate Manifold of Short Hydrogen Bond Arrays Mediating Binding of Active Site-Directed Serine Protease Inhibitors

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU RUH3R
Temperature [K]	285
Detector technology	IMAGE PLATE
Collection date	2002-06-04
Detector	RIGAKU RAXIS IV++
Spacegroup name	C 1 2 1
Unit cell lengths	71.360, 72.060, 72.960
Unit cell angles	90.00, 101.77, 90.00

Refinement procedure

Resolution	7.000 - 1.580
R-factor	0.222
Rwork	0.219
R-free	0.25000
Structure solution method	FOURIER SYNTHESIS
RMSD bond length	0.018
RMSD bond angle	25.600 *
Data reduction software	CrystalClear (1.3)
Data scaling software	CrystalClear ((MSC/RIGAKU))
Refinement software	X-PLOR (3.851)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	32.190	1.650
High resolution limit [Å]	1.380 *	1.580
Rmerge	0.046	0.340 *
Total number of observations	93493 *
Number of reflections	46254 *
<I/σ(I)>	9.6	1.2
Completeness [%]	90.9
Redundancy	2

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	Vapor diffusion, hanging drop *	7 *	298	2-propanol, PEG 4000, pH 6.5, vapor diffusion at 298 K, pH 6.50

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	drop	protein	1.0 (mg/ml)
2	1	drop	HEPES	50 (mM)
3	1	drop	glycerol	50 (%)	pH7.0
4	1	reservoir	HEPES	0.10 (M)
5	1	reservoir		0.30 (M)
6	1	reservoir	PEG5000 MME	22 (%)	pH7.5 or 8.2