EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/06skc0078

Report generated Dec 06, 2006; 13:40:13

Unit cell

1592 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)6.1780 +/- 0.0003
b (Angstrom)7.5785 +/- 0.0003
c (Angstrom)8.0966 +/- 0.0003
alpha (°)100.527 +/- 0.002
beta (°)91.587 +/- 0.003
gamma (°)107.058 +/- 0.003
Volume (A**3)354.97 +/- 0.03
Mosaicity (°)0.631 +/- 0.003

Data collection

Summary

Total number of images collected299
Total exposure time5.1 hours
Data collection exposure time5.0 hours
Data collection wall-clock time5.5 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 collectiont01f51102.0° omega2.000°62 secondsYes
data collectiont02f43 86.0° omega2.000°62 secondsYes
data collectiont03f48 96.0° omega2.000°62 secondsYes
data collectiont04f48 96.0° omega2.000°62 secondsYes
data collectiont05f51102.0° omega2.000°62 secondsYes
data collectiont06f50100.0° omega2.000°62 secondsYes
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected 155
Overload or incomplete profile 226
Sigma cutoff  19
High resolution limit   3

Final Data Set

Scale factor range9.52-19.16
Number of 'full' reflections  3736
Number of 'partial' reflections  3104
Total number of integrated reflections  6523
Total number of unique reflections  1627
Data completeness  98.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  160.5
Average Sigma(I)    3.4
Overall R-merge (linear)  0.050

Sadabs Results

Parameter refinement on 6126 reflections reduced R(int) from 0.0845 to 0.0400

Before rejection, 6456 reflections total and 1633 unique

After rejection, 6086 reflections total and 1630 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.0379   0.854 - 1.265   0.963 - 1.074   2.245    1090    1024
    2   10.2  0.0495   0.883 - 1.128   0.952 - 1.045   2.474     879     826
    3   10.2  0.0335   0.721 - 0.838   0.970 - 1.102   2.189    1010     978
    4   10.2  0.0324   0.713 - 0.900   0.990 - 1.082   2.167    1015     970
    5   10.2  0.0457   0.745 - 1.049   0.989 - 1.085   2.438    1033     960
    6   10.2  0.0372   0.984 - 1.491   0.971 - 1.083   2.170    1059    1004
Ratio of minimum to maximum apparent transmission: 0.864125

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp14 b4  
  Formula   C412H23O5N1  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.1 x 0.1 x 0.04 (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/