EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2005src0328

Report generated Mar 21, 2005; 13:24:46

Unit cell

3163 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)7.7437 +/- 0.0007
b (Angstrom)15.444 +/- 0.002
c (Angstrom)25.704 +/- 0.004
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)3073.9 +/- 0.7
Mosaicity (°)1.169 +/- 0.005

Data collection


Total number of images collected124
Total exposure time197.8 minutes
Data collection exposure time193.8 minutes
Data collection wall-clock time206.6 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance40.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f89178.0° phi2.000°100 secondsYes
data collections02f27 54.0° omega2.000°100 secondsYes
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected 169
Zero sigma or profile test  13
Overload or incomplete profile 724
Sigma cutoff  43
High resolution limit  67

Final Data Set

Scale factor range10.00-11.29
Number of 'full' reflections  4412
Number of 'partial' reflections 11410
Total number of integrated reflections 13657
Total number of unique reflections  3707
Data completeness  93.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   11.1
Average Sigma(I)    1.9
Overall R-merge (linear)  0.173

Sadabs Results

Parameter refinement on 5588 reflections reduced R(int) from 0.1028 to 0.0803

Before rejection, 14823 reflections total and 3851 unique

After rejection, 14544 reflections total and 3850 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.6  0.1824   0.746 - 0.929   0.848 - 2.293   1.374   11923    5109
    2  -12.7  0.1462   0.742 - 0.858   0.855 - 1.151   1.363    2621    1275
Ratio of minimum to maximum apparent transmission: 0.369814


  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. I. R. Butler  
  Local Code   KM 63  
  Formula   C16 H24 N2 Ru1  
  Crystal Colour    Colourless  
  Crystal Habit    Needle  
  Crystal Size   0.18 x 0.03 x 0.02 (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/