5GDS

HIRUNORMS ARE TRUE HIRUDIN MIMETICS. THE CRYSTAL STRUCTURE OF HUMAN ALPHA-THROMBIN:HIRUNORM V COMPLEX

Experimental procedure

Source type	ROTATING ANODE
Source details	RIGAKU RUH2R
Temperature [K]	293
Detector technology	IMAGE PLATE
Collection date	1996-01-10
Detector	RIGAKU RAXIS II
Spacegroup name	C 1 2 1
Unit cell lengths	71.900, 72.800, 73.300
Unit cell angles	90.00, 100.70, 90.00

Refinement procedure

Resolution	20.000 - 2.100
R-factor	0.176 *
Rwork	0.176
Structure solution method	THE STRUCTURE WAS ANALYZED BY DIFFERENCE FOURIER TECHNIQUES
Starting model (for MR)	1HAH (J. VIJAYALAKSHMI ET AL. 1994 PROTEIN SCI. 3 2254-71)
RMSD bond length	0.018
RMSD bond angle	17.835 *
Data reduction software	MOSFLM
Data scaling software	CCP4
Phasing software	CCP4
Refinement software	TNT (5E)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	20.000	2.170
High resolution limit [Å]	2.100	2.100
Rmerge	0.072	0.380
Total number of observations	54776 *
Number of reflections	21615
<I/σ(I)>	5.8	2
Completeness [%]	99.4	98.7
Redundancy	2.5	2.5

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION	7	4 *	THE CRYSTALS OF THROMBIN:HIRUNORM V COMPLEX WERE GROWN, AS DESCRIBED BY SKRZYPEZAK ET AL. (1991) J. MOL. BIOL.,221,1379-1393 BY VAPOR DIFFUSION METHODS AT 4 C. A 6 MICROLITER DROP, CONTAINING 0.05 M SODIUM HEPES (PH 7.0) 10% (W/V) PEG 4000 0.02% NAN3, 20 MG/ML. THROMBIN:HIRUNORM V COMPLEX WAS EQUILIBRATED AGAINST A PRECIPITATING SOLUTION CONTAINING 0.1 M SODIUM HEPES (PH 7.0) 20% (W/V) PEG 4000 0.04% NAN3. CRYSTAL OF THROMBIN:HIRUGEN COMPLEX WERE CRUSHED AND INDIVIDUAL SEEDS WERE USED FOR CROSS-SEEDING EXPERIMENTS., vapor diffusion, temperature 277K

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	drop	sodium Hepes	0.05 (M)
2	1	drop	PEG4000	10 (%(w/v))
3	1	drop		0.02 (%)
4	1	drop	thrombin-hirugen complex	12 (mg/ml)
5	1	reservoir	sodium Hepes	0.1 (M)
6	1	reservoir	PEG4000	20 (%(w/v))
7	1	reservoir		0.04 (%)