EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/07skc0024

Report generated Apr 13, 2007; 10:47:39

Unit cell

2048 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)5.5879 +/- 0.0002
b (Angstrom)22.5846 +/- 0.0012
c (Angstrom)7.3582 +/- 0.0004
alpha (°) 90.000
beta (°)98.580 +/- 0.003
gamma (°) 90.000
Volume (A**3)918.22 +/- 0.08
Mosaicity (°)0.429 +/- 0.002

Data collection


Total number of images collected243
Total exposure time60.3 minutes
Data collection exposure time59.6 minutes
Data collection wall-clock time78.7 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance31.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f203304.5° phi1.500°15 secondsYes
data collections02f32 48.0° omega1.500°15 secondsYes
Phi/Chii01f - i08f85 seconds

Scalepack Scaling

Deleted observations

Rejected  53
Overload or incomplete profile 246
Sigma cutoff  47
High resolution limit   8

Final Data Set

Scale factor range9.21-10.04
Number of 'full' reflections  6631
Number of 'partial' reflections  4380
Total number of integrated reflections  9871
Total number of unique reflections  2159
Data completeness  99.4%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   35.4
Average Sigma(I)    1.7
Overall R-merge (linear)  0.061

Sadabs Results

Parameter refinement on 6451 reflections reduced R(int) from 0.1248 to 0.0502

Before rejection, 10788 reflections total and 2174 unique

After rejection, 10605 reflections total and 2171 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.0618   0.898 - 1.046   0.937 - 1.161   1.204    9164    5984
    2   -7.8  0.0700   0.547 - 0.620   0.937 - 1.153   1.253    1441     955
Ratio of minimum to maximum apparent transmission: 0.806585


  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   WU Maleic 4Meimdz  
  Formula   C8H14O4N2  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.4 x 0.26 x 0.14 (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/