1QB1

Bovine Trypsin with 1-[2-[5-[amino(imino)methyl]-2-hydroxyphenoxy]-6-[3-(4,5-dihydro-1-methyl-1H-imidazol-2-yl)phenoxy]pyridin-4-yl]piperidine-3-carboxylic Acid (ZK-806974)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	SIEMENS
Temperature [K]	297
Detector technology	IMAGE PLATE
Collection date	1995-04-12
Detector	MARRESEARCH
Spacegroup name	P 21 21 21
Unit cell lengths	63.160, 63.780, 69.350
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	10.000 - 1.800
R-factor	0.183 *
Rwork	0.183
R-free	0.23700
Structure solution method	DIRECT REPLACEMENT
RMSD bond length	0.016
RMSD bond angle	0.030
Data reduction software	DENZO
Data scaling software	SCALEPACK
Refinement software	PROFFT

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	10.000	1.900
High resolution limit [Å]	1.800	1.800
Rmerge	0.078 *	0.222 *
Number of reflections	26263
<I/σ(I)>	16.2	3.11
Completeness [%]	99.0	99.9
Redundancy	3.4	3.11

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. REFERENCES 7 (BODE, TURK & STURZEBACHER) AND 8 (BARTUNIK, SUMMERS & BARTSH) HAVE DESCRIBED THE CRYSTALLIZATION OF THE ORTHORHOMBIC FORM OF BOVINE TRYPSIN. CRYSTALS WERE SEEDING INTO DROPS CONTAINING 40 MG/ML BOVINE TRYPSIN, 0.0125 M BENZAMIDINE, 0.7 TO 0.9 M AS, 0.05 M MES PH 6.0, 0.0025 M CACL2 AFTER EQUILIBRATION AGAINST THE CRYSTALLIZATION RESERVOIR FOR 1 DAY. THE CRYSTALLIZATION RESERVOIRS CONTAINED 1.4 TO 1.8 M AS, 0.1 M MES PH 6.0, 0.005 M CACL2., pH 7.4, 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)