EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007src1376

Report generated Oct 20, 2007; 08:17:51

Unit cell

93003 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)5.3320 +/- 0.0004
b (Angstrom)12.9425 +/- 0.0009
c (Angstrom)20.2396 +/- 0.0015
alpha (°)71.806 +/- 0.003
beta (°)89.317 +/- 0.003
gamma (°)78.634 +/- 0.004
Volume (A**3)1299.02 +/- 0.17
Mosaicity (°)2.225 +/- 0.002

Data collection

Summary

Total number of images collected1058
Total exposure time11.8 hours
Data collection exposure time11.8 hours
Data collection wall-clock time12.5 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance40.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f363363.0° phi1.000°40 secondsYes
data collections02f62 62.0° omega1.000°40 secondsYes
data collections03f63 63.0° omega1.000°40 secondsYes
data collections04f62 62.0° omega1.000°40 secondsYes
data collections05f67 67.0° omega1.000°40 secondsYes
data collections06f84 84.0° omega1.000°40 secondsYes
data collections07f115115.0° omega1.000°40 secondsYes
data collections08f121121.0° omega1.000°40 secondsYes
data collections09f113113.0° omega1.000°40 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected   5
Zero sigma or profile test  49
Overload or incomplete profile1814
Sigma cutoff1247
High resolution limit2483

Final Data Set

Scale factor10.00
Number of 'full' reflections     0
Number of 'partial' reflections 21937
Total number of integrated reflections 14711
Total number of unique reflections  5110
Data completeness  89.1%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  271.1
Average Sigma(I)    8.2
Overall R-merge (linear)  0.198

Sadabs Results

Parameter refinement on 22730 reflections reduced R(int) from 0.1830 to 0.0747

Before rejection, 28254 reflections total and 6026 unique

After rejection, 23476 reflections total and 5988 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   18.8  0.0613   0.901 - 1.415   0.842 - 1.272   2.012    8320    6741
    2   18.3  0.0536   0.485 - 0.583   0.917 - 1.336   1.927    1386    1164
    3   18.3  0.0728   0.617 - 0.764   0.829 - 1.131   2.214    1481    1113
    4   18.3  0.0655   0.816 - 1.456   0.828 - 1.230   2.131    1213     952
    5   18.3  0.0616   0.326 - 0.481   0.928 - 1.193   2.042    1598    1317
    6   18.3  0.0739   0.738 - 1.044   0.928 - 1.237   2.093    2005    1586
    7   18.3  0.0771   0.599 - 0.816   0.928 - 1.159   1.980    2772    2255
    8   18.3  0.0746   0.536 - 0.881   0.829 - 1.240   2.083    2639    2055
    9   18.3  0.0669   0.599 - 1.125   0.828 - 1.244   2.076    2062    1643
Ratio of minimum to maximum apparent transmission: 0.619713

Metadata

  Group    Service  
  Operator     
  Sample Owner     
  Local Code   FV HP  
  Formula   C28Hp32N2S4  
  Crystal Colour    Yellow  
  Crystal Habit    Plate  
  Crystal Size   0.2 x 0.1 x 0.005 (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/