EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2009src0245tw

Report generated Mar 17, 2009; 10:19:26

Unit cell

a (Angstrom) 23.7480
b (Angstrom) 6.9040
c (Angstrom) 24.2670
alpha (°) 90.000
beta (°) 93.232
gamma (°) 90.000
Volume (A**3)3972.4

Data collection


Total number of images collected428
Total exposure time35.7 minutes
Data collection exposure time35.1 minutes
Data collection wall-clock time91.7 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance45.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f164196.8° phi1.200°5 secondsYes
data collections02f28 33.6° omega1.200°5 secondsYes
data collections03f116139.2° omega1.200°5 secondsYes
data collections04f112134.4° omega1.200°5 secondsYes
Phi/Chii01f - i08f84 seconds

Scalepack Scaling

Deleted observations

Rejected  36
Zero sigma or profile test  20
Overload or incomplete profile1202
Sigma cutoff  19
High resolution limit  21

Final Data Set

Scale factor10.00
Number of 'full' reflections  5305
Number of 'partial' reflections 38973
Total number of integrated reflections 37538
Total number of unique reflections  9632
Data completeness  97.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   29.8
Average Sigma(I)    2.2
Overall R-merge (linear)  0.132

Sadabs Results

Estimated minimum and maximum transmission: 0.6324 0.7456


  Group    Service  
  Operator   Sam Callear  
  Sample Owner   Prof P.G Taylor  
  Local Code   SM 114bis  
  Formula   C15H17ClN4O6Si  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.37 x 0.31 x 0.19 (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 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    'graphite'
_diffrn_measurement_device_type   'Bruker-Nonius Roper 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. (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/