EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2009src1065

Report generated Oct 05, 2009; 11:49:00

Unit cell

30832 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)7.9832 +/- 0.0006
b (Angstrom)8.8773 +/- 0.0007
c (Angstrom)12.1929 +/- 0.0010
alpha (°)95.866 +/- 0.003
beta (°)107.215 +/- 0.005
gamma (°)114.500 +/- 0.004
Volume (A**3)725.49 +/- 0.11
Mosaicity (°)1.785 +/- 0.004

Data collection

Summary

Total number of images collected351
Total exposure time117.5 minutes
Data collection exposure time116.2 minutes
Data collection wall-clock time131.0 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance31.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f179358.0° phi2.000°20 secondsYes
data collections02f13 26.0° omega2.000°20 secondsYes
data collections03f24 48.0° omega2.000°20 secondsYes
data collections04f52104.0° omega2.000°20 secondsYes
data collections05f24 48.0° omega2.000°20 secondsYes
data collections06f51102.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected   2
Zero sigma or profile test   2
Overload or incomplete profile 628
Sigma cutoff 428
High resolution limit  12

Final Data Set

Scale factor10.00
Number of 'full' reflections   464
Number of 'partial' reflections 15424
Total number of integrated reflections 14014
Total number of unique reflections  3327
Data completeness  98.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   68.4
Average Sigma(I)    2.3
Overall R-merge (linear)  0.073

Sadabs Results

Parameter refinement on 9727 reflections reduced R(int) from 0.0601 to 0.0424

Before rejection, 14540 reflections total and 3347 unique

After rejection, 12793 reflections total and 3325 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.7  0.0476   0.824 - 0.970   0.970 - 1.188   2.112    6879    4573
    2   11.1  0.0461   0.673 - 0.728   0.979 - 1.112   2.075     392     259
    3   11.1  0.0572   0.495 - 0.563   0.976 - 1.046   2.154     815     504
    4   11.1  0.0479   0.721 - 0.903   0.970 - 1.075   2.081    1956    1337
    5   11.1  0.0647   0.685 - 0.793   0.988 - 1.131   2.120     817     517
    6   11.1  0.0479   1.674 - 2.223   0.986 - 1.068   2.096    1934    1233
Ratio of minimum to maximum apparent transmission: 0.816499

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr PJ Murphy  
  Local Code   DME-176-8-10  
  Formula   C12 H18 N3 O3 F3  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Blade  
  Crystal Size   0.12 x 0.08 x 0.05 (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/