Mass: 18.015 Da / Num. of mol.: 34 / Source method: isolated from a natural source / Formula: H2O
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Experimental details
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Experiment
Experiment
Method: X-RAY DIFFRACTION / Number of used crystals: 1
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Sample preparation
Crystal
Density Matthews: 3.99 Å3/Da / Density % sol: 69 % Description: THE STRUCTURE WAS SOLVED USING PB AND OS DERIVATIVE FOR INITIAL PHASING. PHASE EXTENSION WAS PERFORMED WITH THE BEST NATIVE DATA SET
Crystal grow
Details: 5 MG/ML 5-8% /W/V) PEG6000 FROM FLUKA, 0.05-0.2M NACL, 0.1 M CACODYLATE PH 5-6.5
Type: MARRESEARCH / Detector: CCD / Date: Jan 29, 2003
Radiation
Protocol: SINGLE WAVELENGTH / Monochromatic (M) / Laue (L): M / Scattering type: x-ray
Radiation wavelength
Wavelength: 0.801 Å / Relative weight: 1
Reflection
Resolution: 2.8→25 Å / Num. obs: 23384 / % possible obs: 98.5 % / Observed criterion σ(I): 3 / Redundancy: 3.2 % / Rmerge(I) obs: 0.08 / Net I/σ(I): 12.1
Reflection shell
Resolution: 2.8→2.85 Å / Mean I/σ(I) obs: 3
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Processing
Software
Name
Version
Classification
REFMAC
5.8.0107
refinement
DENZO
datareduction
SCALEPACK
datascaling
SOLVE-RESOLVE
phasing
Refinement
Method to determine structure: MIRAS Starting model: NONE Resolution: 2.9→49.26 Å / Cor.coef. Fo:Fc: 0.92 / Cor.coef. Fo:Fc free: 0.878 / SU B: 17.837 / SU ML: 0.328 / Cross valid method: THROUGHOUT / ESU R: 1.666 / ESU R Free: 0.41 / Stereochemistry target values: MAXIMUM LIKELIHOOD Details: HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS. U VALUES REFINED INDIVIDUALLY. HYDROGENS HAVE BEEN USED IF PRESENT IN THE INPUT INITIALY, DOMAINS 4,5 AND 6 COULD BE TRACED ONLY AS POLY- ...Details: HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS. U VALUES REFINED INDIVIDUALLY. HYDROGENS HAVE BEEN USED IF PRESENT IN THE INPUT INITIALY, DOMAINS 4,5 AND 6 COULD BE TRACED ONLY AS POLY- ALA. THE ELECTRON DENSITY OF DOMAINS 4,5 AND 6 WAS NOT GOOD ENOUGH FOR PLACING THE INDIVIDUAL SIDE CHAINS. DOMAIN 6 HAS DISORDERED REGIONS.
Rfactor
Num. reflection
% reflection
Selection details
Rfree
0.274
1218
5.1 %
RANDOM
Rwork
0.22993
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obs
0.23219
22500
89.72 %
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Solvent computation
Ion probe radii: 0.8 Å / Shrinkage radii: 0.8 Å / VDW probe radii: 1.2 Å / Solvent model: MASK