1QB9

BOVINE TRYPSIN 7-[[2-[[1-(1-IMINOETHYL)PIPERIDIN-4-YL]OXY]-9H-CARBOZOL-9-YL] METHYL]NAPHTHALENE-2-CARBOXIMIDAMIDE (ZK-806450) COMPLEX

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU RU300
Temperature [K]	297
Detector technology	IMAGE PLATE
Collection date	1994-12-27
Detector	RIGAKU RAXIS II
Spacegroup name	P 31 2 1
Unit cell lengths	54.510, 54.510, 108.710
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	10.000 - 1.800
R-factor	0.176 *
Rwork	0.176
R-free	0.27800
Structure solution method	DIRECT REPLACEMENT
RMSD bond length	0.016
RMSD bond angle	0.034
Data reduction software	DENZO
Data scaling software	SCALEPACK
Refinement software	PROFFT

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	10.000	2.100
High resolution limit [Å]	1.800	1.800
Rmerge	0.094 *	0.175 *
Number of reflections	10983
<I/σ(I)>	7.9	3.69
Completeness [%]	67.2	71.4
Redundancy	2.83	2.2

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.4	297	MICROCRYSTALS WERE INITIALLY GROWN USING THE HANGING DROP METHOD IN LINBRO CULTURE PLATES. CRYSTALLIZATION RESERVOIRS CONTAIN 1.8 - 2.0 M AMMONIUM SULFATE, 50 MM TRIS HCL, 10 MM CACL2, PH 7.4. SIX UL OF 15 MG/ML BOVINE TRYPSIN IN 20 MM 2-AMINOBENZIMIDAZOLE WAS ADDED TO 6 UL OF RESERVOIR. MACROSEEDING WAS USED TO GROW LARGE CRYSTALS (REF. 5). SINGLE CRYSTALS WERE WASHED IN 0.8 M AMMONIUM SULFATE, 50 MM TRIS HCL, 10 MM CACL2, PH 7.4. THE WASHED CRYSTALS WERE PLACED IN A 18 HOUR OLD HANGING, VAPOR DIFFUSION, HANGING DROP, temperature 297K

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	reservoir	ammonium sulfate	1.8-2.0 (M)
2	1	reservoir	Tris-HCl	50 (mM)
3	1	reservoir		10 (mM)
4	1	drop	trypsin	15 (mg/ml)
5	1	drop	2-aminobenzimidazole	20 (mM)