EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007src0194

Report generated Feb 06, 2007; 07:34:01

Unit cell

2845 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p2
a (Angstrom)6.0473 +/- 0.0004
b (Angstrom)27.1382 +/- 0.0016
c (Angstrom)10.4990 +/- 0.0007
alpha (°) 90.000
beta (°)96.181 +/- 0.003
gamma (°) 90.000
Volume (A**3)1713.0 +/- 0.2
Mosaicity (°)1.575 +/- 0.002

Data collection

Summary

Total number of images collected741
Total exposure time9.2 hours
Data collection exposure time9.2 hours
Data collection wall-clock time9.7 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance45.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f128128.0° omega1.000°45 secondsYes
data collections02f130130.0° omega1.000°45 secondsYes
data collections03f124124.0° omega1.000°45 secondsYes
data collections04f130130.0° omega1.000°45 secondsYes
data collections05f92 92.0° omega1.000°45 secondsYes
data collections06f129129.0° omega1.000°45 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 307
Zero sigma or profile test   9
Overload or incomplete profile1086
Sigma cutoff 474
High resolution limit 318

Final Data Set

Scale factor range8.54-12.11
Number of 'full' reflections     0
Number of 'partial' reflections 17551
Total number of integrated reflections 12241
Total number of unique reflections  3568
Data completeness  89.6%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  167.9
Average Sigma(I)    4.6
Overall R-merge (linear)  0.052

Sadabs Results

Parameter refinement on 17332 reflections reduced R(int) from 0.2179 to 0.0673

Before rejection, 21214 reflections total and 4002 unique

After rejection, 17520 reflections total and 3965 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   10.6  0.0449   0.715 - 0.972   0.917 - 1.105   2.017    2771    2396
    2   21.4  0.0579   0.696 - 1.053   0.944 - 1.345   2.070    3092    2440
    3   21.4  0.0534   0.729 - 0.938   0.912 - 1.260   2.070    3403    2756
    4   21.4  0.0586   0.731 - 1.044   0.917 - 1.105   2.175    2741    2088
    5   21.4  0.0593   0.712 - 0.936   0.972 - 1.213   2.089    1922    1493
    6   21.4  0.0474   0.707 - 0.916   0.911 - 1.162   1.986    3591    2965
Ratio of minimum to maximum apparent transmission: 0.677926

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Davies  
  Local Code   306-310-1  
  Formula   C6H4ClF8N3O2P3  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.1 x 0.06 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 V2.10 (Sheldrick, G.M., 2003)'

_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 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   9.091

_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. (2003). SADABS. Version 2.10. 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/