EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/07skc0009

Report generated Feb 10, 2007; 17:56:50

Unit cell

5578 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p1
a (Angstrom)8.3065 +/- 0.0004
b (Angstrom)10.8557 +/- 0.0008
c (Angstrom)15.6661 +/- 0.0012
alpha (°)71.623 +/- 0.003
beta (°)77.610 +/- 0.004
gamma (°)81.796 +/- 0.004
Volume (A**3)1305.09 +/- 0.16
Mosaicity (°)1.281 +/- 0.003

Data collection

Summary

Total number of images collected321
Total exposure time7.1 hours
Data collection exposure time7.0 hours
Data collection wall-clock time7.2 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance32.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°80 secondsYes
data collections02f13 26.0° omega2.000°80 secondsYes
data collections03f13 26.0° omega2.000°80 secondsYes
data collections04f53106.0° omega2.000°80 secondsYes
data collections05f28 56.0° omega2.000°80 secondsYes
data collections06f25 50.0° omega2.000°80 secondsYes
Phi/Chii01f - i08f840 seconds

Scalepack Scaling

Deleted observations

Rejected 579
Zero sigma or profile test   3
Overload or incomplete profile 780
Sigma cutoff 729
Low resolution limit  12
High resolution limit  53

Final Data Set

Scale factor range10.00-17.73
Number of 'full' reflections  4997
Number of 'partial' reflections 19525
Total number of integrated reflections 21766
Total number of unique reflections  5972
Data completeness  98.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   22.6
Average Sigma(I)    1.4
Overall R-merge (linear)  0.107

Sadabs Results

Parameter refinement on 13063 reflections reduced R(int) from 0.1384 to 0.0695

Before rejection, 23096 reflections total and 6047 unique

After rejection, 19972 reflections total and 5986 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   12.6  0.0880   0.817 - 1.218   0.976 - 1.128   2.083   11890    6549
    2   12.0  0.0880   0.949 - 1.086   0.992 - 1.078   2.012     723     438
    3   12.0  0.0820   0.441 - 0.496   0.995 - 1.111   2.058     690     366
    4   12.0  0.0929   0.759 - 0.966   0.981 - 1.102   2.104    3407    1866
    5   12.0  0.0776   0.476 - 0.597   0.989 - 1.118   1.990    1719    1039
    6   12.0  0.0821   0.531 - 0.609   0.985 - 1.084   2.027    1543     863
Ratio of minimum to maximum apparent transmission: 0.865668

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp16 b11  
  Formula   C12H23O6N1  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.1 x 0.08 x 0.02 (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 V2.10 (Sheldrick, G.M., 2003)'

_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 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   9.091

_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. (2003). SADABS. Version 2.10. 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/