1C2J

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	1998-03-14
Detector	RIGAKU RAXIS IV++
Spacegroup name	P 31 2 1
Unit cell lengths	54.960, 54.960, 109.550
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	7.500 - 1.400
R-factor	0.189
Rwork	0.189
R-free	0.21900
Structure solution method	DIFFERENCE FOURIER PLUS REFINEMENT
RMSD bond length	0.018
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]	35.930	1.460
High resolution limit [Å]	1.330	1.400
Rmerge	0.099	0.328
Number of reflections	28909
<I/σ(I)>	8.1	1.7
Completeness [%]	72.0	34.4
Redundancy	2.5

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	unknown *	7.06		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 100 NM ZN(II), PH 7.06 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.