EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/07skc0018

Report generated Feb 18, 2007; 08:35:45

Unit cell

2235 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)6.6307 +/- 0.0004
b (Angstrom)11.5496 +/- 0.0007
c (Angstrom)22.2265 +/- 0.0010
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)1702.15 +/- 0.16
Mosaicity (°)0.871 +/- 0.003

Data collection


Total number of images collected196
Total exposure time49.4 minutes
Data collection exposure time48.0 minutes
Data collection wall-clock time55.7 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance36.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f121181.5° phi1.500°15 secondsYes
data collections02f67100.5° omega1.500°15 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 405
Zero sigma or profile test   5
Overload or incomplete profile 356
Sigma cutoff 142
High resolution limit  14

Final Data Set

Scale factor range7.22-10.89
Number of 'full' reflections  3259
Number of 'partial' reflections  8967
Total number of integrated reflections 11321
Total number of unique reflections  2268
Data completeness  99.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   32.9
Average Sigma(I)    1.1
Overall R-merge (linear)  0.085

Sadabs Results

Parameter refinement on 8757 reflections reduced R(int) from 0.1434 to 0.0643

Before rejection, 11945 reflections total and 2281 unique

After rejection, 10325 reflections total and 2274 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.9  0.0691   0.708 - 1.237   0.944 - 1.162   2.045    6633    4639
    2   15.4  0.0639   0.600 - 0.789   0.950 - 1.255   1.999    3692    2693
Ratio of minimum to maximum apparent transmission: 0.752785


  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp8 f5  
  Formula   C13H31O4N1  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.18 x 0.1 x 0.04 (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/