1C2I

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	1997-02-25
Detector	RIGAKU RAXIS IV++
Spacegroup name	P 31 2 1
Unit cell lengths	55.000, 55.000, 109.760
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	7.500 - 1.470
R-factor	0.177
Rwork	0.177
R-free	0.20800
Structure solution method	DIFFERENCE FOURIER PLUS REFINEMENT
RMSD bond length	0.019
RMSD bond angle	4.000
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]	54.800	1.540
High resolution limit [Å]	1.400	1.470
Rmerge	0.071	0.225
Number of reflections	27202
<I/σ(I)>	12.7	2
Completeness [%]	80.0	34.4
Redundancy	3.2

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	unknown *	5.5		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 46 MM ZN(II), PH 5.50 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.