EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2008lsh022r

Report generated Jul 07, 2008; 16:41:09

Unit cell

26360 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)9.2339 +/- 0.0003
b (Angstrom)11.9540 +/- 0.0004
c (Angstrom)13.4630 +/- 0.0004
alpha (°)64.5016 +/- 0.0018
beta (°)87.652 +/- 0.002
gamma (°)76.670 +/- 0.002
Volume (A**3)1302.31 +/- 0.08
Mosaicity (°)0.799 +/- 0.002

Data collection

Summary

Total number of images collected331
Total exposure time143.7 minutes
Data collection exposure time141.7 minutes
Data collection wall-clock time160.5 minutes

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 collections01f50100.0° omega2.000°26 secondsYes
data collections02f44 88.0° omega2.000°26 secondsYes
data collections03f34 68.0° omega2.000°26 secondsYes
data collections04f51102.0° omega2.000°26 secondsYes
data collections05f46 92.0° omega2.000°26 secondsYes
data collections06f50100.0° omega2.000°26 secondsYes
data collections07f48 96.0° omega2.000°26 secondsYes
Phi/Chii01f - i08f815 seconds

Scalepack Scaling

Deleted observations

Rejected   3
Overload or incomplete profile1030
Sigma cutoff 510
High resolution limit  54

Final Data Set

Scale factor10.00
Number of 'full' reflections 12759
Number of 'partial' reflections 15649
Total number of integrated reflections 25769
Total number of unique reflections  5965
Data completeness  99.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   62.7
Average Sigma(I)    2.0
Overall R-merge (linear)  0.166

Sadabs Results

Parameter refinement on 18108 reflections reduced R(int) from 0.1300 to 0.0461

Before rejection, 26177 reflections total and 6005 unique

After rejection, 22896 reflections total and 5966 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    6.7  0.0483   0.831 - 1.214   0.961 - 1.120   2.046    3616    2572
    2   10.2  0.0495   0.917 - 1.152   0.954 - 1.123   2.043    3106    2139
    3   10.2  0.0509   0.683 - 1.010   0.960 - 1.129   2.148    2352    1550
    4   10.2  0.0492   0.817 - 1.517   0.954 - 1.082   2.070    3636    2562
    5   10.2  0.0508   0.631 - 0.939   0.961 - 1.214   2.044    3232    2252
    6   10.2  0.0541   0.822 - 1.081   0.976 - 1.115   2.028    3555    2490
    7   10.2  0.0620   0.454 - 0.684   0.977 - 1.133   2.125    3399    2119
Ratio of minimum to maximum apparent transmission: 0.785466

Metadata

  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   PMC/OCH3  
  Formula   C9 H11 N1 O3  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Plate  
  Crystal Size   0.3 x 0.01 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 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/