EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/05src0006

Report generated Jan 12, 2005; 09:09:13

Unit cell

3723 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)6.2659 +/- 0.0003
b (Angstrom)10.0140 +/- 0.0006
c (Angstrom)14.6666 +/- 0.0008
alpha (°)70.827 +/- 0.002
beta (°)85.930 +/- 0.004
gamma (°)72.323 +/- 0.003
Volume (A**3)827.77 +/- 0.08
Mosaicity (°)0.620 +/- 0.003

Data collection

Summary

Total number of images collected324
Total exposure time15.2 hours
Data collection exposure time14.9 hours
Data collection wall-clock time15.3 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance32.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°170 secondsYes
data collections02f16 32.0° omega2.000°170 secondsYes
data collections03f16 32.0° omega2.000°170 secondsYes
data collections04f24 48.0° omega2.000°170 secondsYes
data collections05f55110.0° omega2.000°170 secondsYes
data collections06f24 48.0° omega2.000°170 secondsYes
Phi/Chii01f - i08f8120 seconds

Scalepack Scaling

Deleted observations

Rejected  76
Zero sigma or profile test   6
Overload or incomplete profile 612
Sigma cutoff  23
High resolution limit  25

Final Data Set

Scale factor range4.32-10.47
Number of 'full' reflections  9987
Number of 'partial' reflections  7895
Total number of integrated reflections 17179
Total number of unique reflections  3787
Data completeness  99.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   54.3
Average Sigma(I)    2.9
Overall R-merge (linear)  0.087

Sadabs Results

Parameter refinement on 8239 reflections reduced R(int) from 0.1460 to 0.0533

Before rejection, 16635 reflections total and 3802 unique

After rejection, 16298 reflections total and 3797 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.3  0.0648   0.915 - 1.078   0.895 - 1.168   1.299    9425    5749
    2   -8.7  0.1035   0.760 - 0.827   0.952 - 1.059   1.357     764     394
    3   -8.7  0.1172   0.421 - 0.460   0.899 - 1.062   1.396     748     357
    4   -8.7  0.1390   0.542 - 0.700   0.943 - 1.062   1.515    1207     485
    5   -8.7  0.0684   0.889 - 1.120   0.925 - 1.063   1.305    2941    1647
    6   -8.7  0.1728   0.954 - 1.055   0.896 - 1.150   1.507    1213     452
Ratio of minimum to maximum apparent transmission: 0.766336

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr A. K. Croft  
  Local Code   AG206  
  Formula   C21 H22 O2  
  Crystal Colour    Colourless  
  Crystal Habit    Rod  
  Crystal Size   0.09 x 0.03 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/