EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2007jmw0002

Report generated Feb 27, 2007; 14:24:09

Unit cell

1605 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p2
a (Angstrom)10.0114 +/- 0.0009
b (Angstrom)4.3352 +/- 0.0003
c (Angstrom)16.6163 +/- 0.0014
alpha (°) 90.000
beta (°)106.2907 +/- 0.0018
gamma (°) 90.000
Volume (A**3)692.22 +/- 0.10
Mosaicity (°)0.456 +/- 0.002

Data collection

Summary

Total number of images collected595
Total exposure time53.4 minutes
Data collection exposure time52.0 minutes
Data collection wall-clock time76.6 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance60.20 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f234234.0° phi1.000°5 secondsYes
data collections02f85 85.0° omega1.000°5 secondsYes
data collections03f160160.0° omega1.000°5 secondsYes
data collections04f108108.0° omega1.000°5 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 225
Overload or incomplete profile 170
Sigma cutoff  11
High resolution limit  38

Final Data Set

Scale factor range8.32-14.70
Number of 'full' reflections  2850
Number of 'partial' reflections  3288
Total number of integrated reflections  5741
Total number of unique reflections  1741
Data completeness  97.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   47.4
Average Sigma(I)    1.6
Overall R-merge (linear)  0.070

Sadabs Results

Parameter refinement on 4657 reflections reduced R(int) from 0.1709 to 0.0558

Before rejection, 6169 reflections total and 1774 unique

After rejection, 5633 reflections total and 1768 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1  -22.7  0.0588   0.575 - 1.148   0.952 - 1.168   2.058    1990    1509
    2   28.5  0.0609   0.372 - 0.552   0.952 - 1.179   1.970     877     681
    3   28.5  0.0514   0.866 - 1.098   0.951 - 1.090   1.896    1669    1296
    4   28.5  0.0578   1.031 - 2.118   0.940 - 1.060   1.965    1097     827
Ratio of minimum to maximum apparent transmission: 0.796896

Metadata

  Group    Academic  
  Operator   Mike Hursthouse  
  Sample Owner   JMW  
  Local Code   CC4780422  
  Formula   C7H8O3S1  
  Crystal Colour    Colourless  
  Crystal Habit    Lath  
  Crystal Size   0.25 x 0.06 x 0.01 (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    '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

_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/