1C2K

RECRUITING ZINC TO MEDIATE POTENT, SPECIFIC INHIBITION OF SERINE PROTEASES

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Temperature [K]	298
Detector technology	IMAGE PLATE
Collection date	1997-01-13
Detector	RIGAKU RAXIS IV++
Spacegroup name	P 31 2 1
Unit cell lengths	54.910, 54.910, 108.930
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	7.500 - 1.650
R-factor	0.202
Rwork	0.202
R-free	0.24300
Structure solution method	DIFFERENCE FOURIER PLUS REFINEMENT
RMSD bond length	0.018
RMSD bond angle	3.900
Data reduction software	bioteX ((MSC))
Data scaling software	bioteX
Phasing software	X-PLOR
Refinement software	X-PLOR (3.1)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	43.580	1.720
High resolution limit [Å]	1.450	1.650
Rmerge	0.082	0.270
Number of reflections	17380
<I/σ(I)>	6.4	1.6
Completeness [%]	68.0	32.8
Redundancy	2.9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	unknown *	3.85		BATCH, 1.51 M MGSO4 . 7 H2O, 0.59 MM TRYPSIN, 1.0 MM ZN(II) 5.0 % DMSO: CRYSTALLIZATION SOLUTION WAS SATURATED IN KETO-BABIM. CRYSTAL WAS TRANSFERRED TO SYNTHETIC MOTHER LIQUOR CONTAINING 2.11 M ZN(II), PH 3.85 AND SOAKED FOR SEVERAL DAYS WITH SEVERAL REPLACEMENTS OF SOAKING SOLUTIONS. THE SOLUTION WAS SATURATED IN KETO-BABIM AND CONTAINED 2.0 % DMSO TO INCREASE INHIBITOR SOLUBILITY. UNDER THIS CONDITION KETO-BABIM UNDERGOES DECOMPOSITION TO 5- AMIDINO-BENZIMIDAZOLE.