EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2005src1570

Report generated Dec 02, 2005; 16:31:18

Unit cell

8343 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)11.3931 +/- 0.0004
b (Angstrom)12.6750 +/- 0.0004
c (Angstrom)13.6059 +/- 0.0004
alpha (°)72.140 +/- 0.002
beta (°)78.9205 +/- 0.0017
gamma (°)82.034 +/- 0.002
Volume (A**3)1828.57 +/- 0.10
Mosaicity (°)1.129 +/- 0.002

Data collection

Summary

Total number of images collected405
Total exposure time81.9 minutes
Data collection exposure time80.8 minutes
Data collection wall-clock time113.1 minutes

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°12 secondsYes
data collections02f56112.0° omega2.000°12 secondsYes
data collections03f24 48.0° omega2.000°12 secondsYes
data collections04f56112.0° omega2.000°12 secondsYes
data collections05f24 48.0° omega2.000°12 secondsYes
data collections06f56112.0° omega2.000°12 secondsYes
Phi/Chii01f - i08f88 seconds

Scalepack Scaling

Deleted observations

Rejected 238
Zero sigma or profile test   4
Overload or incomplete profile1996
Sigma cutoff  41
High resolution limit  33

Final Data Set

Scale factor range7.97-17.24
Number of 'full' reflections 14068
Number of 'partial' reflections 36458
Total number of integrated reflections 47588
Total number of unique reflections  8401
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   53.3
Average Sigma(I)    1.9
Overall R-merge (linear)  0.062

Sadabs Results

Parameter refinement on 30231 reflections reduced R(int) from 0.1087 to 0.0489

Before rejection, 47324 reflections total and 8415 unique

After rejection, 46773 reflections total and 8415 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.3  0.0613   0.772 - 1.119   0.927 - 1.157   1.372   21386   14074
    2   -8.7  0.0519   0.680 - 1.088   0.927 - 1.084   1.283    6642    4907
    3   -8.7  0.0641   0.869 - 0.980   0.974 - 1.084   1.373    2665    1850
    4   -8.7  0.0611   0.697 - 0.888   0.978 - 1.092   1.327    6703    4521
    5   -8.7  0.0590   0.806 - 0.913   0.974 - 1.161   1.335    2685    1907
    6   -8.7  0.0601   0.709 - 1.088   0.927 - 1.155   1.362    6692    4374
Ratio of minimum to maximum apparent transmission: 0.798607

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. N. Greeves  
  Local Code   386/1  
  Formula   C20 H30 O1  
  Crystal Colour    Colourless  
  Crystal Habit    Slab  
  Crystal Size   0.38 x 0.17 x 0.08 (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/