EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/06skc0018

Report generated Jun 09, 2006; 08:13:17

Unit cell

3834 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p1
a (Angstrom)5.8667 +/- 0.0007
b (Angstrom)13.738 +/- 0.002
c (Angstrom)15.427 +/- 0.002
alpha (°)64.386 +/- 0.006
beta (°)90.012 +/- 0.009
gamma (°)90.085 +/- 0.010
Volume (A**3)1121.2 +/- 0.3
Mosaicity (°)2.862 +/- 0.006

Data collection

Summary

Total number of images collected334
Total exposure time5.5 hours
Data collection exposure time5.5 hours
Data collection wall-clock time6.0 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance35.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°60 secondsYes
data collections02f16 32.0° omega2.000°60 secondsYes
data collections03f27 54.0° omega2.000°60 secondsYes
data collections04f27 54.0° omega2.000°60 secondsYes
data collections05f16 32.0° omega2.000°60 secondsYes
data collections06f59118.0° omega2.000°60 secondsYes
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected 208
Zero sigma or profile test   7
Overload or incomplete profile1438
Sigma cutoff 108
High resolution limit 205

Final Data Set

Scale factor range5.13-11.36
Number of 'full' reflections     0
Number of 'partial' reflections 20099
Total number of integrated reflections 16651
Total number of unique reflections  4665
Data completeness  91.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   28.1
Average Sigma(I)    3.4
Overall R-merge (linear)  0.123

Sadabs Results

Parameter refinement on 9502 reflections reduced R(int) from 0.1225 to 0.0715

Before rejection, 19816 reflections total and 5092 unique

After rejection, 19254 reflections total and 5087 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0934   1.153 - 1.895   0.909 - 1.300   1.363   10866    6297
    2  -11.2  0.1883   0.351 - 0.411   0.964 - 1.246   1.451     830     362
    3  -11.2  0.1340   0.395 - 0.469   0.949 - 1.293   1.480    1550     847
    4  -11.2  0.2097   0.321 - 0.376   0.933 - 1.251   1.553    1538     699
    5  -11.2  0.1718   0.371 - 0.446   0.927 - 1.186   1.515     821     376
    6  -11.2  0.1523   1.204 - 1.559   0.908 - 1.178   1.450    3649    1861
Ratio of minimum to maximum apparent transmission: 0.698721

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp6 b4  
  Formula   C8H15O4N1S1  
  Crystal Colour    Colourless  
  Crystal Habit    Shard  
  Crystal Size   0.08 x 0.05 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/