Mass: 18.015 Da / Num. of mol.: 75 / 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: 4
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Sample preparation
Crystal
Density Matthews: 2.42 Å3/Da / Density % sol: 49.14 % Description: MAD PHASE FROM THE INCORPORATED PT WAS COMBINED WITH MIR PHASES FROM BR AND PT DERIVATIVES.
Crystal grow
pH: 7.5 Details: 0.1 M HEPES (PH 7.5), 0.05 M K2HPO4, 10% (W/V) PEG 8000 WITH 25% GYLCEROL AS CRYOPROTECTANT
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Data collection
Diffraction
ID
Mean temperature (K)
Crystal-ID
1
100
1
2
1
Diffraction source
Source
Site
Beamline
ID
Wavelength (Å)
SYNCHROTRON
SSRL
BL9-2
1
0.85, 2.06
SYNCHROTRON
SSRL
BL9-1
2
0.77, 0.98
Detector
Type
ID
Detector
Date
MARMOSAIC 325 mm CCD
1
CCD
Jan 21, 2008
ADSC CCD
2
CCD
Radiation
ID
Protocol
Monochromatic (M) / Laue (L)
Scattering type
Wavelength-ID
1
SINGLEWAVELENGTH
M
x-ray
1
2
SINGLEWAVELENGTH
M
x-ray
1
Radiation wavelength
ID
Wavelength (Å)
Relative weight
1
0.85
1
2
2.06
1
3
0.77
1
4
0.98
1
Reflection
Resolution: 2.4→30 Å / Num. obs: 17143 / % possible obs: 92.9 % / Observed criterion σ(I): 5 / Redundancy: 3.1 % / Rmerge(I) obs: 0.03 / Net I/σ(I): 32
Reflection shell
Resolution: 2.4→2.49 Å / Redundancy: 3 % / Rmerge(I) obs: 0.33 / Mean I/σ(I) obs: 4.3 / % possible all: 95.7
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Processing
Software
Name
Version
Classification
DENZO
datareduction
SCALEPACK
datascaling
SOLVE
phasing
RESOLVE
phasing
REFMAC
5.2.0019
refinement
Refinement
Method to determine structure: MIRAS Starting model: NONE Resolution: 2.4→29.1 Å / Cor.coef. Fo:Fc: 0.945 / Cor.coef. Fo:Fc free: 0.914 / SU B: 14.435 / SU ML: 0.169 / TLS residual ADP flag: LIKELY RESIDUAL / Cross valid method: THROUGHOUT / ESU R: 0.375 / ESU R Free: 0.251 / Stereochemistry target values: MAXIMUM LIKELIHOOD Details: HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS. RESIDUES 57-67,108-112,170-175,208-212 IN CHAIN A AND 61- 68,100-106,172-174,205-212 IN CHAIN B ARE DISORDERED
Rfactor
Num. reflection
% reflection
Selection details
Rfree
0.245
914
5.1 %
RANDOM
Rwork
0.209
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obs
0.211
17143
94.1 %
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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: BABINET MODEL WITH MASK