Mass: 18.015 Da / Num. of mol.: 73 / 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: 2.43 Å3/Da / Density % sol: 49.47 % / Description: NONE
Crystal grow
Temperature: 293 K / Method: vapor diffusion, sitting drop Details: CRYSTALS WERE GROWN IN SITTING DROPS AT 20 C. VPS33A-HIS10 (200 NL; 3.2 MG/ML) WAS EQUILIBRATED AGAINST 80 UL RESERVOIRS CONTAINING 14.3-12.8% (W/V) PEG 3350 AND 143-128 MM AMMONIUM ACETATE ...Details: CRYSTALS WERE GROWN IN SITTING DROPS AT 20 C. VPS33A-HIS10 (200 NL; 3.2 MG/ML) WAS EQUILIBRATED AGAINST 80 UL RESERVOIRS CONTAINING 14.3-12.8% (W/V) PEG 3350 AND 143-128 MM AMMONIUM ACETATE (HAMPTON RESEARCH). CRYSTALS WERE CRYOPROTECTED BY ADDING RESERVOIR SOLUTION SUPPLEMENTED WITH 30% (V/V) ETHYLENE GLYCOL TO THE MOTHER LIQUOR IMMEDIATELY BEFORE HARVESTING AND CRYO-COOLING BY PLUNGING INTO LIQUID NITROGEN. ANNEALING BY BLOCKING THE CRYOSTREAM FOR 5 S GREATLY ENHANCED THE DIFFRACTION OF VPS33A CRYSTALS.
Type: DECTRIS PILATUS 6M / Detector: PIXEL / Date: May 20, 2011 Details: KIRKPATRICK BAEZ BIMORPH MIRROR PAIR FOR HORIZONTAL AND VERTICAL FOCUSSING
Radiation
Monochromator: DOUBLE CRYSTAL / Protocol: SINGLE WAVELENGTH / Monochromatic (M) / Laue (L): M / Scattering type: x-ray
Radiation wavelength
Wavelength: 0.9763 Å / Relative weight: 1
Reflection
Resolution: 2.4→64.5 Å / Num. obs: 49915 / % possible obs: 96.9 % / Observed criterion σ(I): -3 / Redundancy: 3.5 % / Biso Wilson estimate: 53.776 Å2 / Rmerge(I) obs: 0.09 / Net I/σ(I): 9.5
Reflection shell
Resolution: 2.4→2.49 Å / Redundancy: 3.6 % / Rmerge(I) obs: 0.77 / Mean I/σ(I) obs: 1.7 / % possible all: 97.8
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Processing
Software
Name
Version
Classification
REFMAC
5.7.0029
refinement
XDS
datareduction
XSCALE
datascaling
autoSHARP
phasing
Refinement
Method to determine structure: MIRAS Starting model: NONE Resolution: 2.4→64.61 Å / Cor.coef. Fo:Fc: 0.95 / Cor.coef. Fo:Fc free: 0.929 / SU B: 18.921 / SU ML: 0.204 / Cross valid method: THROUGHOUT / ESU R: 0.438 / ESU R Free: 0.263 / Stereochemistry target values: MAXIMUM LIKELIHOOD Details: HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS. U VALUES WITH TLS ADDED
Rfactor
Num. reflection
% reflection
Selection details
Rfree
0.24377
2103
4.2 %
RANDOM
Rwork
0.19721
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obs
0.19914
47789
96.45 %
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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