EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2007src0238

Report generated Feb 14, 2007; 14:50:26

Unit cell

11225 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)7.23190 +/- 0.00010
b (Angstrom)11.0720 +/- 0.0003
c (Angstrom)18.1646 +/- 0.0005
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)1454.47 +/- 0.06
Mosaicity (°)0.4830 +/- 0.0010

Data collection


Total number of images collected179
Total exposure time59.0 minutes
Data collection exposure time57.6 minutes
Data collection wall-clock time71.2 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f148296.0° phi2.000°20 secondsYes
data collections02f23 46.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 121
Overload or incomplete profile 480
Sigma cutoff  29
High resolution limit  13

Final Data Set

Scale factor range9.65-10.68
Number of 'full' reflections 11985
Number of 'partial' reflections  6208
Total number of integrated reflections 16753
Total number of unique reflections  1937
Data completeness  99.4%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  203.4
Average Sigma(I)    3.7
Overall R-merge (linear)  0.037

Sadabs Results

Parameter refinement on 15873 reflections reduced R(int) from 0.0652 to 0.0338

Before rejection, 17666 reflections total and 3374 unique

After rejection, 17431 reflections total and 3371 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0347   0.914 - 1.026   0.955 - 1.138   1.414   15196   13936
    2    6.8  0.0349   0.790 - 0.859   0.953 - 1.090   1.416    2235    2094
Ratio of minimum to maximum apparent transmission: 0.837440


  Group    Service  
  Operator   Louise Male  
  Sample Owner   Dr P. G. Taylor  
  Local Code   SB0607  
  Formula   C13 H21 N1 O2 Si1  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.4 x 0.4 x 0.34 (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    'graphite'
_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/