EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/04skc0013

Report generated Feb 09, 2005; 14:46:40

Unit cell

2627 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
a (Angstrom)8.1489 +/- 0.0003
b (Angstrom)9.5095 +/- 0.0004
c (Angstrom)14.3941 +/- 0.0006
alpha (°) 90.000
beta (°)94.380 +/- 0.002
gamma (°) 90.000
Volume (A**3)1112.17 +/- 0.08
Mosaicity (°)0.576 +/- 0.002

Data collection


Total number of images collected205
Total exposure time134.7 minutes
Data collection exposure time132.0 minutes
Data collection wall-clock time147.3 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance32.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f143286.0° phi2.000°40 secondsYes
data collections02f54108.0° omega2.000°40 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected  63
Overload or incomplete profile 476
Sigma cutoff   2
High resolution limit  38

Final Data Set

Scale factor range8.98-13.89
Number of 'full' reflections  8804
Number of 'partial' reflections  6102
Total number of integrated reflections 14450
Total number of unique reflections  2706
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   50.7
Average Sigma(I)    1.8
Overall R-merge (linear)  0.058

Sadabs Results

Parameter refinement on 9375 reflections reduced R(int) from 0.1079 to 0.0461

Before rejection, 14337 reflections total and 2722 unique

After rejection, 14183 reflections total and 2722 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.3  0.0555   0.812 - 1.150   0.926 - 1.225   1.361   10253    7022
    2   -8.7  0.0540   0.610 - 0.952   0.951 - 1.172   1.342    3930    2780
Ratio of minimum to maximum apparent transmission: 0.755465


  Group    Mike Hursthouse  
  Operator   Sam Callear (skc)  
  Sample Owner     
  Local Code   TLT374D G11  
  Formula   C8H17O6N1  
  Crystal Colour    Colourless  
  Crystal Habit    Fragment  
  Crystal Size   0.14 x 0.08 x 0.03 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   85 (mA) 
  Primary Solvent     
  Other Solvents     

File Explanations

      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

'COLLECT (Hooft, R.W.W., 1998)'
'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
'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/