EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/06skc0076

Report generated Nov 27, 2006; 14:32:20

Unit cell

3305 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)4.9228 +/- 0.0002
b (Angstrom)11.3727 +/- 0.0005
c (Angstrom)14.0935 +/- 0.0006
alpha (°)82.683 +/- 0.003
beta (°)90.021 +/- 0.003
gamma (°)89.993 +/- 0.003
Volume (A**3)782.61 +/- 0.06
Mosaicity (°)1.223 +/- 0.002

Data collection

Summary

Total number of images collected563
Total exposure time5.1 hours
Data collection exposure time299.0 minutes
Data collection wall-clock time5.4 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 collections01f102102.0° omega1.000°32 secondsYes
data collections02f98 98.0° omega1.000°32 secondsYes
data collections03f96 96.0° omega1.000°32 secondsYes
data collections04f96 96.0° omega1.000°32 secondsYes
data collections05f95 95.0° omega1.000°32 secondsYes
data collections06f68 68.0° omega1.000°32 secondsYes
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected 495
Zero sigma or profile test  11
Overload or incomplete profile 522
Sigma cutoff 339
High resolution limit  59

Final Data Set

Scale factor range8.64-15.41
Number of 'full' reflections     0
Number of 'partial' reflections 13872
Total number of integrated reflections 12247
Total number of unique reflections  3554
Data completeness  98.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   41.1
Average Sigma(I)    1.6
Overall R-merge (linear)  0.085

Sadabs Results

Parameter refinement on 9636 reflections reduced R(int) from 0.1053 to 0.0592

Before rejection, 13731 reflections total and 3616 unique

After rejection, 12224 reflections total and 3594 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   10.7  0.0652   0.557 - 0.898   0.982 - 1.213   2.159    2254    1528
    2    9.1  0.0625   0.525 - 0.765   0.943 - 1.097   2.028    2227    1630
    3    9.9  0.0710   1.044 - 1.386   0.953 - 1.091   2.115    2092    1422
    4   10.2  0.0606   0.919 - 1.363   0.963 - 1.193   2.022    2127    1556
    5   10.2  0.0560   0.919 - 1.237   0.976 - 1.149   2.034    2064    1467
    6   10.2  0.0703   0.903 - 1.197   0.973 - 1.077   2.093    1460     971
Ratio of minimum to maximum apparent transmission: 0.777306

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp15 d12  
  Formula   C11H22O4N2S1  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.13 x 0.09 x 0.02 (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/