1W2Z

PSAO and Xenon

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU RU200
Temperature [K]	100
Detector technology	IMAGE PLATE
Collection date	2004-01-30
Detector	MAR scanner 345 mm plate
Spacegroup name	P 1 21 1
Unit cell lengths	89.507, 196.268, 89.665
Unit cell angles	90.00, 107.46, 90.00

Refinement procedure

Resolution	29.880 - 2.240
R-factor	0.181
Rwork	0.179
R-free	0.22400
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1ksi
RMSD bond length	0.012
RMSD bond angle	1.322
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	MOLREP
Refinement software	REFMAC (5.1.24)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	29.820	2.300
High resolution limit [Å]	2.240	2.240
Rmerge	0.070	0.170
Number of reflections	141039
<I/σ(I)>	17	7.7
Completeness [%]	99.8	98.9
Redundancy	4.75	4.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.2	293	HANGING DROP VAPOR DIFFUSION AT 293K. RESERVOIR WAS 20% PEG 3350, 0.28M KI. DROPS WERE 2 MICROL OF PSAO AT 21.58MG/ML IN 0.1M KPO4 PH 7.2, PLUS 1 MICROL OF 0.1M KPO4 PH 7.5, PLUS 1 MICROL OF RESERVOIR SOLUTION. THE CRYSTAL WAS CRYOPROTECTED BY SOAKING FOR 5 MIN IN 5 MICROL OF 0.2M KI, 25% PEG 3350 AND 15% GLYCEROL UNDER 30MICROL OF PARAFFIN IN A SITTING DROP DEPRESSION. THE CRYSTAL WAS EXPOSED TO XENON GAS FOR 5 MINUTES, INITIALLY AT PRESSURE OF 100 PSI THEN INCREASING TO A FINAL PRESSURE OF 220 PSI, USING A XENON CHAMBER (HAMPTON RESEARCH). AFTER THE XENON WAS RELEASED FROM THE CHAMBER, THE CRYSTAL WAS SNAP-FROZEN IN LIQUID NITROGEN WITHIN 1-3 S.