EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007may0017

Report generated Sep 30, 2007; 11:19:07

Unit cell

61666 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p222
a (Angstrom)7.8484 +/- 0.0006
b (Angstrom)8.3983 +/- 0.0007
c (Angstrom)24.1255 +/- 0.0018
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)1590.2 +/- 0.2
Mosaicity (°)2.068 +/- 0.003

Data collection

Summary

Total number of images collected767
Total exposure time9.6 hours
Data collection exposure time9.6 hours
Data collection wall-clock time10.1 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 collections01f363363.0° phi1.000°45 secondsYes
data collections02f27 27.0° omega1.000°45 secondsYes
data collections03f55 55.0° omega1.000°45 secondsYes
data collections04f55 55.0° omega1.000°45 secondsYes
data collections05f27 27.0° omega1.000°45 secondsYes
data collections06f72 72.0° omega1.000°45 secondsYes
data collections07f56 56.0° omega1.000°45 secondsYes
data collections08f104104.0° omega1.000°45 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected  12
Zero sigma or profile test 127
Overload or incomplete profile1974
Sigma cutoff1009
High resolution limit  38

Final Data Set

Scale factor10.00
Number of 'full' reflections     0
Number of 'partial' reflections 14731
Total number of integrated reflections  9445
Total number of unique reflections  1556
Data completeness  72.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  197.8
Average Sigma(I)    5.3
Overall R-merge (linear)  0.249

Sadabs Results

Parameter refinement on 16439 reflections reduced R(int) from 0.3275 to 0.0822

Before rejection, 21991 reflections total and 2110 unique

After rejection, 17116 reflections total and 2098 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.1  0.0630   0.582 - 1.748   0.806 - 1.274   2.026    9256    6583
    2   14.6  0.0643   0.258 - 0.308   0.951 - 1.201   2.031     608     471
    3   14.6  0.0736   0.299 - 0.366   0.768 - 1.240   2.040    1062     798
    4   14.6  0.0672   0.497 - 0.654   0.818 - 1.201   2.066    1014     749
    5   14.6  0.1232   0.344 - 0.443   0.803 - 1.240   2.226     323     196
    6   14.6  0.0741   1.038 - 2.570   0.768 - 1.238   2.301     855     614
    7   14.6  0.0678   0.550 - 0.763   0.768 - 1.197   2.224     998     674
    8   14.6  0.0754   0.330 - 1.109   0.928 - 1.275   2.088    3000    2107
Ratio of minimum to maximum apparent transmission: 0.602185

Metadata

  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   cc 01409  
  Formula   C9 H10 O3  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Shard  
  Crystal Size   0.1 x 0.08 x 0.02 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   75 (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 2007/2 (Sheldrick, G.M., 2007)'

_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 APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

_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. (2007). SADABS. Version 2007/2. 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/