EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/05thg021

Report generated Feb 14, 2005; 16:36:27

Unit cell

2766 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)5.5581 +/- 0.0004
b (Angstrom)16.0410 +/- 0.0010
c (Angstrom)11.7863 +/- 0.0006
alpha (°) 90.061
beta (°)103.363 +/- 0.004
gamma (°) 90.033
Volume (A**3)1022.39 +/- 0.11
Mosaicity (°)0.827 +/- 0.004

Data collection


Total number of images collected123
Total exposure time27.4 minutes
Data collection exposure time25.3 minutes
Data collection wall-clock time33.6 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f54108.0° omega2.000°14 secondsYes
data collections02f53106.0° omega2.000°14 secondsYes
Phi/Chii01f - i08f810 seconds
Phi/Chij01f - j08f85 seconds

Scalepack Scaling

Deleted observations

Rejected  14
Overload or incomplete profile 412
Sigma cutoff   6
High resolution limit   6

Final Data Set

Scale factor range6.56-21.51
Number of 'full' reflections  3743
Number of 'partial' reflections  4916
Total number of integrated reflections  8056
Total number of unique reflections  3939
Data completeness  84.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   76.9
Average Sigma(I)    3.8
Overall R-merge (linear)  0.047

Sadabs Results

Parameter refinement on 6315 reflections reduced R(int) from 0.1348 to 0.0429

Before rejection, 8021 reflections total and 2261 unique

After rejection, 7935 reflections total and 2259 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   -3.5  0.0617   1.148 - 2.035   0.892 - 1.165   1.404    4017    3138
    2   -2.5  0.0372   0.536 - 0.799   0.903 - 1.049   1.203    3918    3577
Ratio of minimum to maximum apparent transmission: 0.766173


  Group    Service  
  Sample Owner     
  Local Code     
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.2 x 0.2 x 0.2 (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/