EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2006src0700

Report generated Jun 02, 2006; 12:12:17

Unit cell

3618 reflections with 1.00°<theta<27.48° (resolution between 20.40A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
a (Angstrom)12.2802 +/- 0.0004
b (Angstrom)13.0289 +/- 0.0004
c (Angstrom)18.0335 +/- 0.0005
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)2885.31 +/- 0.15
Mosaicity (°)1.080 +/- 0.002

Data collection


Total number of images collected295
Total exposure time25.3 minutes
Data collection exposure time24.7 minutes
Data collection wall-clock time49.5 minutes

Experimental Conditions

Wavelength0.71073 A


TypeName# imagesTotal
Per frame
per frame
Used in
cell determinationi01f10 10.0° phi1.000°3 seconds45.00 mmNo
data collections01f182182.0° phi1.000°5 seconds32.00 mmYes
data collections02f103103.0° omega1.000°5 seconds32.00 mmYes

Scalepack Scaling

Deleted observations

Rejected 332
Zero sigma or profile test   6
Overload or incomplete profile1212
Sigma cutoff  92
High resolution limit 113

Final Data Set

Scale factor range7.17-10.31
Number of 'full' reflections     0
Number of 'partial' reflections 25581
Total number of integrated reflections 22722
Total number of unique reflections  3688
Data completeness  99.6%
Resolution range20.40-0.77 A
Theta range1.00°-27.48°
Average Intensity   88.6
Average Sigma(I)    3.2
Overall R-merge (linear)  0.069

Sadabs Results

Parameter refinement on 16838 reflections reduced R(int) from 0.2337 to 0.0517

Before rejection, 26430 reflections total and 3728 unique

After rejection, 25767 reflections total and 3726 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.3  0.0569   0.846 - 1.437   0.714 - 1.798   1.238   16577   11308
    2   -8.7  0.0619   0.523 - 0.755   0.716 - 1.413   1.251    9190    6140
Ratio of minimum to maximum apparent transmission: 0.396965


  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Davies  
  Local Code   306-133-a  
  Formula   C3H4BrCl4N4O4P3  
  Crystal Colour    Colourless  
  Crystal Habit    Slab  
  Crystal Size   0.5 x 0.25 x 0.1 (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/