1PAU

Crystal structure of the complex of apopain with the tetrapeptide aldehyde inhibitor AC-DEVD-CHO

Experimental procedure

Source type	ROTATING ANODE
Source details	RIGAKU RUH2R
Temperature [K]	293
Detector technology	AREA DETECTOR
Collection date	1995-11-09
Detector	SIEMENS
Spacegroup name	I 2 2 2
Unit cell lengths	69.810, 84.620, 96.790
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	20.000 - 2.500
R-factor	0.195
Rwork	0.195
R-free	0.27500
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	PROTEIN COMPONENT OF INTERLEUKIN-1BETA CONVERTING ENZYME (PDB ENTRY 1ICE)
RMSD bond length	0.007
RMSD bond angle	24.140 *
Data reduction software	SAINT
Data scaling software	SAINT
Phasing software	X-PLOR (3.1)
Refinement software	X-PLOR (3.1)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	36.000	2.590
High resolution limit [Å]	2.500	2.500
Rmerge	0.055 *	0.257
Total number of observations	20801 *
Number of reflections	8929
<I/σ(I)>	17.4	2.59
Completeness [%]	87.1	87.1
Redundancy	2.33	2.27

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	8.5 *		HANGING DROP VAPOR DIFFUSION. 1.5 MICROLITER DROPS OF PROTEIN:INHIBITOR SOLUTION (8.7 MG/ML IN 10 MILLIMOLAR TRIS-HCL PH 8.5, 10 MILLIMOLAR DTT, 3 MILLIMOLAR SODIUM AZIDE) WERE MIXED WITH AN EQUAL VOLUME OF RESERVOIR BUFFER (7% PEG-6000 (W/W), 0.10 MOLAR SODIUM CITRATE PH 5.0, 10 MILLIMOLAR DTT, 3 MILLIMOLAR SODIUM AZIDE) AND INCUBATED AT ROOM TEMPERATURE, vapor diffusion - hanging drop

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	drop	protein	8.7 (mg/ml)
2	1	drop	Tris-HCl	10 (mM)
3	1	drop	dithiothreitol	10 (mM)
4	1	drop		3 (mM)
5	1	reservoir	PEG6000	7.5 (%(w/w))
6	1	reservoir	sodium citrate	0.10 (M)
7	1	reservoir	dithiothreitol	10 (mM)
8	1	reservoir		3 (mM)