X-RAY DIFFRACTION

Crystallization Details
Method pH Temprature Details
X-RAY DIFFRACTION 8.5 293.15 Samples were centrifuged at 13,000 x g for 3 min to remove macro-aggregates and dust, and crystallised inside an anaerobic chamber (N2/H2 (97:3%) atmosphere, 20 degree Celsius). Crystallisation was done by the sitting drop method in 96-Well MRC 2-Drop polystyrene Crystallisation Plates (SWISSCI) containing 90 uL of crystallisation solution in the reservoir. Crystals were obtained by mixing 0.7 uL of crystallisation solution with 0.7 uL of protein sample at 22.4 mg.ml-1. The crystallisation solution contained the following: 30 % v/v 2-methyl-2,4-pentanediol, 100 mM Tris pH 8.5, 500 mM Sodium chloride and 8 % w/v Polyethylene glycol 8,000 (Crystallisation solution of the JBScreen Wizard form Jena Bioscience, Germany).
Unit Cell:
a: 68.504 Å b: 80.243 Å c: 105.744 Å α: 74.49° β: 82.25° γ: 65.02°
Symmetry:
Space Group: P 1
Crystal Properties:
Matthew's Coefficient: 2.40 Solvent Content: 48.76
Refinement Statistics
Diffraction ID Structure Solution Method Cross Validation Method Resolution Limit (High) Resolution Limit (Low) Number of Reflections (Observed) Number of Reflections (R-free) Percent Reflections (Observed) R-Work R-Free Mean Isotropic
X-RAY DIFFRACTION MOLECULAR REPLACEMENT FREE R-VALUE 1.21 33.62 371077 18775 61.95 0.1221 0.1460 17.71
Data Collection
Overall
Resolution Limit (High) Resolution Limit (Low) Percent Possible (Observed) R Merge I (Observed) R Sym I (Observed) Net I Over Average Sigma (I) Redundancy Number Reflections (All) Number Reflections (Observed) Observed Criterion Sigma (F) Observed Criterion Sigma (I) B (Isotropic) From Wilson Plot
1.21 101.86 92.0 0.074 ? 12.9 7.1 ? 371908 ? ? ?
Highest Resolution Shell
# Resolution Limits (Low) Resolution Limits (High) Percent Possible (All) Percent Possible (Observed) R-Sym I (Observed) Mean I Over Sigma (Observed) Redundancy Number Unique Reflections (All)
1 1.21 1.35 74.5 ? ? 1.7 7.3 ?
Diffraction
Diffraction experiment
Crystal ID Scattering Type Data Collection Temprature Detector Detector Type Details Collection Date Monochromator Protocol
1 100 K ?
Radiation Source
Source Type Wavelength List Synchrotron Site Beamline
SYNCHROTRON ESRF BEAMLINE BM07 0.97951 ESRF BM07
Software
Software Name Purpose Version
PHENIX refinement (1.21.2_5419: ???)
PDB_EXTRACT data extraction .
autoPROC data reduction .
autoPROC data scaling .
PHASER phasing .
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