EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)


Summary report for Directory: diska/2005src0648

Report generated May 17, 2005; 13:10:40

Unit cell

1886 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p222
a (Angstrom)9.9925 +/- 0.0002
b (Angstrom)11.5568 +/- 0.0002
c (Angstrom)12.4480 +/- 0.0003
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)1437.51 +/- 0.05
Mosaicity (°)0.3860 +/- 0.0010

Data collection

Summary

Total number of images collected157
Total exposure time60.7 minutes
Data collection exposure time60.1 minutes
Data collection wall-clock time72.2 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 collections01f79158.0° phi2.000°24 secondsYes
data collections02f16 32.0° omega2.000°24 secondsYes
data collections03f54108.0° omega2.000°24 secondsYes
Phi/Chii01f - i08f84 seconds

Scalepack Scaling

Deleted observations

Rejected  81
Zero sigma or profile test   4
Overload or incomplete profile 440
Sigma cutoff   7

Final Data Set

Scale factor range9.75-12.58
Number of 'full' reflections 11230
Number of 'partial' reflections  4514
Total number of integrated reflections 15232
Total number of unique reflections  1894
Data completeness  99.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  194.2
Average Sigma(I)    3.4
Overall R-merge (linear)  0.028

Sadabs Results

Parameter refinement on 12432 reflections reduced R(int) from 0.0578 to 0.0267

Before rejection, 14870 reflections total and 1896 unique

After rejection, 14711 reflections total and 1891 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0256   0.962 - 1.023   0.966 - 1.124   1.345    7944    6690
    2   -7.1  0.0271   0.756 - 0.808   0.965 - 1.079   1.370    1418    1236
    3   -6.8  0.0288   0.917 - 1.138   0.966 - 1.129   1.279    5349    4602
Ratio of minimum to maximum apparent transmission: 0.855228

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Davies  
  Local Code   305-130-B  
  Formula   C5H10Cl4N3O2P3  
  Crystal Colour    Colourless  
  Crystal Habit    Rod  
  Crystal Size   0.6 x 0.15 x 0.13 (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    'graphite'
_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/