EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/04skc0003

Report generated Jul 19, 2004; 13:26:10

Unit cell

3411 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)13.2850 +/- 0.0016
b (Angstrom)13.2397 +/- 0.0010
c (Angstrom)17.668 +/- 0.002
alpha (°) 90.000
beta (°)106.410 +/- 0.005
gamma (°) 90.000
Volume (A**3)2981.0 +/- 0.5
Mosaicity (°)0.573 +/- 0.005

Data collection


Total number of images collected155
Total exposure time101.2 minutes
Data collection exposure time98.5 minutes
Data collection wall-clock time112.3 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f113226.0° phi2.000°40 secondsYes
data collections02f34 68.0° omega2.000°40 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Zero sigma or profile test  15
Overload or incomplete profile 372
Sigma cutoff  10
High resolution limit  73

Final Data Set

Scale factor range9.87-10.31
Number of 'full' reflections  8482
Number of 'partial' reflections  5976
Total number of integrated reflections 14049
Total number of unique reflections  3517
Data completeness  99.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity    5.7
Average Sigma(I)    0.9
Overall R-merge (linear)  0.225

Sadabs Results

Parameter refinement on 6558 reflections reduced R(int) from 0.3938 to 0.0875

Before rejection, 15461 reflections total and 3553 unique

After rejection, 12222 reflections total and 3363 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.1995   1.040 - 1.249   0.832 - 1.222   1.489    9514    3736
    2   -6.8  0.1904   0.470 - 0.536   0.853 - 1.153   1.443    2708    1146
Ratio of minimum to maximum apparent transmission: 0.680606


  Group    Mike Hursthouse  
  Operator   Suzanna Ward  
  Sample Owner     
  Local Code   TLT374c cd34  
  Formula   C8H19O6N1  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.2 x 0.12 x 0.03 (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/