EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/04skc0001

Report generated Jul 16, 2004; 21:31:50

Unit cell

1871 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)25.128 +/- 0.009
b (Angstrom)4.9921 +/- 0.0009
c (Angstrom)19.255 +/- 0.007
alpha (°) 90.000
beta (°)129.425 +/- 0.008
gamma (°) 90.000
Volume (A**3)1865.8 +/- 1.0
Mosaicity (°)1.155 +/- 0.011

Data collection


Total number of images collected117
Total exposure time227.8 minutes
Data collection exposure time218.4 minutes
Data collection wall-clock time229.2 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f93186.0° phi2.000°120 secondsYes
data collections02f16 32.0° omega2.000°120 secondsYes
Phi/Chii01f - i08f870 seconds

Scalepack Scaling

Deleted observations

Rejected  38
Zero sigma or profile test 308
Overload or incomplete profile 194
Sigma cutoff 118
High resolution limit  12

Final Data Set

Scale factor range10.00-10.58
Number of 'full' reflections  1991
Number of 'partial' reflections  5522
Total number of integrated reflections  6805
Total number of unique reflections  2239
Data completeness  93.4%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity    4.5
Average Sigma(I)    1.2
Overall R-merge (linear)  0.177

Sadabs Results

Parameter refinement on 1610 reflections reduced R(int) from 0.0793 to 0.0547

Before rejection, 6695 reflections total and 2266 unique

After rejection, 6575 reflections total and 2263 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.2120   0.892 - 1.029   0.777 - 1.797   1.234    5728    1820
    2   -6.8  0.1737   0.696 - 0.737   0.686 - 1.335   1.160     847     285
Ratio of minimum to maximum apparent transmission: 0.381797


  Group    Mike Hursthouse  
  Operator   Suzanna Ward  
  Sample Owner     
  Local Code   TLT374D E11  
  Formula   C7H10O6N2  
  Crystal Colour    Colourless  
  Crystal Habit    Fragment  
  Crystal Size   0.09 x 0.08 x 0.06 (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. SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10

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/