1HW7

HSP33, HEAT SHOCK PROTEIN WITH REDOX-REGULATED CHAPERONE ACTIVITY

Experimental procedure

Experimental method	MAD
Source type	SYNCHROTRON
Source details	APS BEAMLINE 14-BM-C
Synchrotron site	APS
Beamline	14-BM-C
Temperature [K]	100
Detector technology	CCD
Collection date	2000-03-31
Detector	ADSC QUANTUM 4
Wavelength(s)	1.0
Spacegroup name	P 65 2 2
Unit cell lengths	77.180, 77.180, 199.210
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	30.000 - 2.200
R-factor	0.229 *
Rwork	0.230
R-free	0.25670
Structure solution method	MAD
Starting model (for MR)	Structure phased by three-wavelength MAD experiment of AUCN-derived crystals and refined to 2.4 A.
RMSD bond length	0.015
RMSD bond angle	1.900
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	SOLVE
Refinement software	CNS (0.9)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	30.000	2.280
High resolution limit [Å]	2.200	2.200
Rmerge	0.048	0.323
Total number of observations	444763 *
Number of reflections	18629
<I/σ(I)>	45.7	14
Completeness [%]	99.7	99.9
Redundancy	23.9	6.9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.5 *	22 *	Drops contained 2 microlitres of protein solution (10mg/ml in 20mM KCL, 40mM HEPES pH 7.5) supplemented with 2mM DTT and 0.3 mM ZnCl2 and 2 microlitres of precipitant (1.5 M ammonium sulfate, 10% dioxane, 0.1 M MES pH 6.8) and were equilibrated against 1ml of the same precipitant., VAPOR DIFFUSION, HANGING DROP, temperature 298K

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	drop	protein	10 (mg/ml)
2	1	drop		20 (mM)
3	1	drop	HEPES	40 (mM)
4	1	drop	dithiothreitol	20 (mM)
5	1	reservoir	ammonium sulfate	1.5 (M)
6	1	reservoir	dioxane	10 (%)
7	1	reservoir	MES	0.1 (M)