EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2009skc0160

Report generated Feb 17, 2009; 11:38:24

Unit cell

12672 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p2
a (Angstrom)11.5592 +/- 0.0004
b (Angstrom)11.4724 +/- 0.0004
c (Angstrom)12.1273 +/- 0.0003
alpha (°) 90.000
beta (°)90.735 +/- 0.002
gamma (°) 90.000
Volume (A**3)1608.09 +/- 0.09
Mosaicity (°)0.472 +/- 0.002

Data collection

Summary

Total number of images collected218
Total exposure time29.8 minutes
Data collection exposure time29.1 minutes
Data collection wall-clock time39.5 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f45 90.0° omega2.000°8 secondsYes
data collections02f51102.0° omega2.000°8 secondsYes
data collections03f48 96.0° omega2.000°8 secondsYes
data collections04f24 48.0° omega2.000°8 secondsYes
data collections05f42 84.0° omega2.000°8 secondsYes
Phi/Chii01f - i08f85 seconds

Scalepack Scaling

Deleted observations

Rejected   3
Zero sigma or profile test  16
Overload or incomplete profile 608
Sigma cutoff 240
High resolution limit  12

Final Data Set

Scale factor10.00
Number of 'full' reflections 14884
Number of 'partial' reflections  7938
Total number of integrated reflections 21831
Total number of unique reflections  3872
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   19.9
Average Sigma(I)    0.7
Overall R-merge (linear)  0.179

Sadabs Results

Parameter refinement on 13620 reflections reduced R(int) from 0.0911 to 0.0602

Before rejection, 21172 reflections total and 3884 unique

After rejection, 18069 reflections total and 3870 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    4.8  0.0737   0.809 - 0.983   0.963 - 1.108   2.037    4050    2462
    2   10.5  0.0615   0.655 - 0.851   0.814 - 1.117   1.976    4404    2849
    3   10.2  0.0690   0.851 - 0.941   0.960 - 1.116   1.956    4113    2654
    4   10.2  0.0962   0.611 - 0.874   0.918 - 1.117   2.142    1965     936
    5   10.2  0.0670   0.834 - 0.932   0.954 - 1.108   1.999    3537    2163
Ratio of minimum to maximum apparent transmission: 0.729191

Metadata

  Group    Personal  
  Operator   Sam Callear  
  Sample Owner   Dr SK Callear  
  Local Code   2 (diol)  
  Formula   C7H16O2  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.18 x 0.09 x 0.05 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   85 (mA) 
  Primary Solvent     
  Other Solvents     

File Explanations

SampleCode.zip
      SampleCode.hkl - data corrected using  SADABS
      SampleCode_merge_none.hkl - equivalents and friedels kept separate  (See "Final Data Set" table in this report)
      SampleCode.p4p - skeleton p4p file for use with XPREP
      SampleCode.htm - this summary file


Southampton CIF entry fields

_exptl_absorpt_process_details       'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type   'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 

Software References

Unit Cell Determination using DirAx:
Duisenberg AJM. Indexing in Single-Crystal Diffractometry with an Obstinate List of Reflections. Journal of Applied Crystallography 1992; 25: 92-96.
Duisenberg AJM, Hooft RWW, Schreurs AMM, Kroon J. Accurate cells from area-detector images. Journal of Applied Crystallography 2000; 33: 893-898.

Diffractometer control and strategy calculation using COLLECT:
Hooft RWW. COLLECT data collection software, Nonius B.V., 1998.

Standard Data Reduction using HKL(Denzo & Scalepack):
Otwinowski Z, Minor W. Processing of X-ray diffraction data collected in oscillation mode. Macromolecular Crystallography, Pt A. 1997; 276: 307-326.

Absorption Correction
Sheldrick, G. M. (2007). SADABS. Version 2007/2. Bruker AXS Inc., Madison, Wisconsin, USA.

Non-Standard Data Reduction using EvalCCD:
Duisenberg AJM, Kroon-Batenburg LMJ, Schreurs AMM. An intensity evaluation method: EVAL-14. Journal of Applied Crystallography 2003; 36: 220-229.

For more information visit the service web site at: http://www.soton.ac.uk/~xservice/