EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2008lsh115

Report generated Nov 06, 2008; 15:43:38

Unit cell

14167 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
c2
a (Angstrom)20.7183 +/- 0.0007
b (Angstrom)12.6104 +/- 0.0005
c (Angstrom)9.1726 +/- 0.0003
alpha (°) 90.000
beta (°)109.300 +/- 0.002
gamma (°) 90.000
Volume (A**3)2261.81 +/- 0.14
Mosaicity (°)0.685 +/- 0.002

Data collection

Summary

Total number of images collected228
Total exposure time75.9 minutes
Data collection exposure time74.5 minutes
Data collection wall-clock time122.2 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 collections01f45 90.0° omega2.000°20 secondsYes
data collections02f51102.0° omega2.000°20 secondsYes
data collections03f48 96.0° omega2.000°20 secondsYes
data collections04f31 62.0° omega2.000°20 secondsYes
data collections05f45 90.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected   2
Overload or incomplete profile 468
Sigma cutoff 250
High resolution limit  14

Final Data Set

Scale factor10.00
Number of 'full' reflections  8719
Number of 'partial' reflections  8155
Total number of integrated reflections 15843
Total number of unique reflections  2705
Data completeness 100.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   75.2
Average Sigma(I)    1.8
Overall R-merge (linear)  0.145

Sadabs Results

Parameter refinement on 11550 reflections reduced R(int) from 0.1256 to 0.0499

Before rejection, 15546 reflections total and 2714 unique

After rejection, 13699 reflections total and 2709 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    3.9  0.0527   0.902 - 1.125   0.983 - 1.101   2.081    2869    2128
    2   10.2  0.0527   0.546 - 1.134   0.978 - 1.074   2.030    3176    2350
    3   10.2  0.0528   0.955 - 1.280   0.978 - 1.077   2.090    2966    2083
    4   10.2  0.0595   0.473 - 0.529   0.983 - 1.136   2.048    1880    1386
    5   10.2  0.0476   0.798 - 1.141   0.978 - 1.140   2.030    2808    1989
Ratio of minimum to maximum apparent transmission: 0.858081

Metadata

  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   MMC/F  
  Formula   C8 H8 F1 N1 O2  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Lath  
  Crystal Size   0.26 x 0.08 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/