1C3M

CRYSTAL STRUCTURE OF HELTUBA COMPLEXED TO MAN(1-3)MAN

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU RU200
Temperature [K]	298
Detector technology	IMAGE PLATE
Collection date	1998-07-20
Detector	MARRESEARCH
Spacegroup name	I 4 2 2
Unit cell lengths	106.373, 106.373, 65.099
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	15.000 - 2.350 *
Rwork	0.171
R-free	0.21700
RMSD bond length	0.015
RMSD bond angle	26.800 *
Data reduction software	DENZO
Data scaling software	CCP4 ((SCALA))
Phasing software	CNS
Refinement software	CNS

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	15.000	2.450
High resolution limit [Å]	2.350	2.350
Rmerge	0.087	0.395
Total number of observations	60741 *
Number of reflections	7889
<I/σ(I)>	7.6
Completeness [%]	98.5	95.2 *
Redundancy	4.9	3.8

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION	7	20 *	26-28% PEG 550 monomethyl ester 0.2 M magnesium acetate, pH 7.0, VAPOR DIFFUSION, temperature 298K

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	drop	protein	2.5 (mg/ml)
2	1	drop	HEPES	10 (mM)
3	1	drop		150 (mM)
4	1	drop	EDTA	3 (mM)
5	1	drop	p20	0.005 (%)
6	1	reservoir	mPEG550	26-28 (%)
7	1	reservoir	calcium acetate	0.2 (M)	or magnesium acetate
8	1	reservoir	HEPES	0.1 (M)