EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/06skc0020

Report generated Jun 15, 2006; 23:36:43

Unit cell

1300 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)5.6944 +/- 0.0002
b (Angstrom)7.1036 +/- 0.0004
c (Angstrom)23.7560 +/- 0.0012
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)960.95 +/- 0.08
Mosaicity (°)0.490 +/- 0.003

Data collection


Total number of images collected221
Total exposure time203.6 minutes
Data collection exposure time199.5 minutes
Data collection wall-clock time228.8 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance35.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f135189.0° phi1.400°56 secondsYes
data collections02f78109.2° omega1.400°56 secondsYes
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected  43
Zero sigma or profile test   1
Overload or incomplete profile 298
Sigma cutoff   9
High resolution limit   6

Final Data Set

Scale factor range9.05-10.48
Number of 'full' reflections  4581
Number of 'partial' reflections  4206
Total number of integrated reflections  8500
Total number of unique reflections  1334
Data completeness  99.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   25.5
Average Sigma(I)    1.3
Overall R-merge (linear)  0.100

Sadabs Results

Parameter refinement on 5335 reflections reduced R(int) from 0.0907 to 0.0671

Before rejection, 8427 reflections total and 1338 unique

After rejection, 8277 reflections total and 1338 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0864   1.278 - 1.557   0.917 - 1.265   1.387    5142    3485
    2   -6.9  0.0965   0.471 - 0.575   0.941 - 1.207   1.396    3135    2064
Ratio of minimum to maximum apparent transmission: 0.724298


  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/