Mass: 18.015 Da / Num. of mol.: 396 / Source method: isolated from a natural source / Formula: H2O
Nonpolymer details
CALCIUM ION (CA): CA2+ IONS FROM CRYSTALLIZATION SOLUTION. POSITION VERIFIED BY ANOMALOUS ...CALCIUM ION (CA): CA2+ IONS FROM CRYSTALLIZATION SOLUTION. POSITION VERIFIED BY ANOMALOUS DIFFERENCE DENSITY. IDENTITY INFERRED FROM SURROUNDINGS. CHLORIDE ION (CL): CL- IONS FROM CRYSTALLIZATION SOLUTION. POSITION VERIFIED BY ANOMALOUS DIFFERENCE DENSITY. IDENTITY INFERRED FROM SURROUNDINGS.
Sequence details
FIRST THREE RESIDUES GAM DERIVE FROM TEV CLEAVAGE OF GST TAG.
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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: 2.03 Å3/Da / Density % sol: 39.3 % Description: DATA MERGED FROM THREE DIFFERENT WAVELENGTHS COLLECTED FROM THE SAME CRYSTAL. 0.81 A COLLECTED ON X11 WITH FLATPANEL DETECTOR. 0.95 A AND 1.9 A COLLECTED ON X12 WITH MAR 225 CCD DETECTOR.
Crystal grow
Temperature: 293 K / Method: vapor diffusion Details: 20 DEG C IN HANGING OR SITTING-DROPS WITH 2 UL PROTEIN (17.3 MG/ML) PLUS 1 UL RESERVOIR (0.1 M NA-ACETATE PH 5.0, 0.2 M CACL2, 18 % PEG 6000).
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Data collection
Diffraction
ID
Mean temperature (K)
Crystal-ID
1
100
1
2
100
1
Diffraction source
Source
Site
Beamline
ID
Wavelength
SYNCHROTRON
EMBL/DESY, HAMBURG
X11
1
0.81
SYNCHROTRON
EMBL/DESY, HAMBURG
X12
2
Detector
Type
ID
Detector
MAR555 FLAT PANEL
1
IMAGE PLATE
MARMOSAIC 225 mm CCD
2
CCD
Radiation
ID
Protocol
Monochromatic (M) / Laue (L)
Scattering type
Wavelength-ID
1
MAD
M
x-ray
1
2
M
x-ray
1
Radiation wavelength
Wavelength: 0.81 Å / Relative weight: 1
Reflection
Resolution: 1.3→47 Å / Num. obs: 66287 / % possible obs: 99.9 % / Observed criterion σ(I): -3 / Redundancy: 22.7 % / Biso Wilson estimate: 21 Å2 / Rmerge(I) obs: 0.07 / Net I/σ(I): 31.8
Reflection shell
Resolution: 1.3→1.33 Å / Rmerge(I) obs: 0.72 / Mean I/σ(I) obs: 2.98 / % possible all: 99.3
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Processing
Software
Name
Version
Classification
REFMAC
5.5.0109
refinement
XDS
datareduction
XSCALE
datascaling
SHELXD
phasing
Refinement
Method to determine structure: MAD Starting model: NONE Resolution: 1.3→47 Å / Cor.coef. Fo:Fc: 0.974 / Cor.coef. Fo:Fc free: 0.964 / SU B: 2.556 / SU ML: 0.047 / Cross valid method: THROUGHOUT / ESU R: 0.057 / ESU R Free: 0.055 / Stereochemistry target values: MAXIMUM LIKELIHOOD Details: HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS. U VALUES REFINED INDIVIDUALLY
Rfactor
Num. reflection
% reflection
Selection details
Rfree
0.19559
1989
3 %
RANDOM
Rwork
0.15709
-
-
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obs
0.15827
64294
99.9 %
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Solvent computation
Ion probe radii: 0.8 Å / Shrinkage radii: 0.8 Å / VDW probe radii: 1.4 Å / Solvent model: BABINET MODEL WITH MASK