EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007src1054

Report generated Aug 03, 2007; 14:07:21

Unit cell

16164 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)9.7504 +/- 0.0003
b (Angstrom)10.2281 +/- 0.0003
c (Angstrom)14.0530 +/- 0.0005
alpha (°)95.766 +/- 0.002
beta (°)107.8415 +/- 0.0015
gamma (°)96.617 +/- 0.002
Volume (A**3)1311.46 +/- 0.07
Mosaicity (°)0.524 +/- 0.002

Data collection

Summary

Total number of images collected376
Total exposure time64.0 minutes
Data collection exposure time63.3 minutes
Data collection wall-clock time87.2 minutes

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 collections01f181362.0° phi2.000°10 secondsYes
data collections02f13 26.0° omega2.000°10 secondsYes
data collections03f13 26.0° omega2.000°10 secondsYes
data collections04f27 54.0° omega2.000°10 secondsYes
data collections05f27 54.0° omega2.000°10 secondsYes
data collections06f52104.0° omega2.000°10 secondsYes
data collections07f55110.0° omega2.000°10 secondsYes
Phi/Chii01f - i08f85 seconds

Scalepack Scaling

Deleted observations

Zero sigma or profile test  12
Overload or incomplete profile 874
Sigma cutoff 342
High resolution limit  19

Final Data Set

Scale factor10.00
Number of 'full' reflections 16560
Number of 'partial' reflections  9738
Total number of integrated reflections 24764
Total number of unique reflections  6024
Data completeness  99.4%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   37.2
Average Sigma(I)    1.4
Overall R-merge (linear)  0.203

Sadabs Results

Parameter refinement on 16695 reflections reduced R(int) from 0.1392 to 0.0541

Before rejection, 24597 reflections total and 6039 unique

After rejection, 21431 reflections total and 6002 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.1  0.0668   0.576 - 1.411   0.986 - 1.142   2.116   10737    6953
    2   14.6  0.0512   1.284 - 1.352   0.994 - 1.106   2.082     635     434
    3   14.6  0.0544   0.755 - 0.841   0.983 - 1.077   2.025     663     462
    4   14.6  0.0441   1.225 - 1.386   0.986 - 1.073   1.894    1535    1171
    5   14.6  0.0445   0.641 - 0.837   0.983 - 1.053   1.970    1550    1147
    6   14.6  0.0524   1.171 - 1.636   0.988 - 1.147   1.981    3053    2102
    7   14.6  0.0623   0.453 - 0.528   0.983 - 1.094   2.043    3258    2120
Ratio of minimum to maximum apparent transmission: 0.857568

Metadata

  Group    Service  
  Operator   Louise Male  
  Sample Owner   Dr John Spencer  
  Local Code   Sami acetone  
  Formula   C11 H11 N1 O1  
  Crystal Colour    Pale Orange  
  Crystal Habit    Plate  
  Crystal Size   0.3 x 0.08 x 0.04 (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/