EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)


Summary report for Directory: diska/2005src0807

Report generated Jun 23, 2005; 08:33:43

Unit cell

2154 reflections with 2.91°<theta<27.10° (resolution between 7.00A and 0.78A) were used for unit cell refinement

Symmetry used
in scalepack
p222
a (Angstrom)8.2989 +/- 0.0008
b (Angstrom)11.7171 +/- 0.0008
c (Angstrom)19.1591 +/- 0.0018
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)1863.0 +/- 0.3
Mosaicity (°)1.820 +/- 0.003

Data collection

Summary

Total number of images collected214
Total exposure time8.1 hours
Data collection exposure time8.0 hours
Data collection wall-clock time8.3 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f171171.0° phi1.000°140 secondsYes
data collections02f35 35.0° omega1.000°140 secondsYes
Phi/Chii01f - i08f850 seconds

Scalepack Scaling

Deleted observations

Rejected  93
Zero sigma or profile test  12
Overload or incomplete profile 728
Sigma cutoff  43

Final Data Set

Scale factor range9.61-18.02
Number of 'full' reflections     0
Number of 'partial' reflections 13372
Total number of integrated reflections 11808
Total number of unique reflections  2313
Data completeness  97.5%
Resolution range7.00-0.78 A
Theta range2.91°-27.10°
Average Intensity   39.6
Average Sigma(I)    2.1
Overall R-merge (linear)  0.077

Sadabs Results

Parameter refinement on 8248 reflections reduced R(int) from 0.0807 to 0.0537

Before rejection, 13258 reflections total and 2370 unique

After rejection, 12999 reflections total and 2367 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    6.4  0.0813   0.823 - 1.070   0.714 - 1.561   1.347   10963    7168
    2   -5.8  0.0579   0.720 - 0.784   0.671 - 1.252   1.192    2036    1595
Ratio of minimum to maximum apparent transmission: 0.429813

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Cunningham  
  Local Code   STS-020  
  Formula   C20H16NO2Cl2  
  Crystal Colour    Colourless  
  Crystal Habit    Shard  
  Crystal Size   0.24 x 0.08 x 0.06 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   85 (mA) 
  Primary Solvent     
  Other Solvents     

File Explanations

SampleCode.zip
      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

_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'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
_computing_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/