EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/06skc0053

Report generated Sep 11, 2006; 07:26:01

Unit cell

2929 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)8.1962 +/- 0.0004
b (Angstrom)8.1974 +/- 0.0004
c (Angstrom)10.5044 +/- 0.0005
alpha (°)95.175 +/- 0.003
beta (°)95.169 +/- 0.003
gamma (°)111.778 +/- 0.003
Volume (A**3)646.87 +/- 0.06
Mosaicity (°)0.683 +/- 0.003

Data collection

Summary

Total number of images collected369
Total exposure time6.1 hours
Data collection exposure time6.0 hours
Data collection wall-clock time6.6 hours

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 collections01f181362.0° phi2.000°60 secondsYes
data collections02f16 32.0° omega2.000°60 secondsYes
data collections03f55110.0° omega2.000°60 secondsYes
data collections04f23 46.0° omega2.000°60 secondsYes
data collections05f31 62.0° omega2.000°60 secondsYes
data collections06f55110.0° omega2.000°60 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected 519
Zero sigma or profile test   3
Overload or incomplete profile 676
Sigma cutoff  12
High resolution limit 142

Final Data Set

Scale factor range5.06-12.59
Number of 'full' reflections  8551
Number of 'partial' reflections  7822
Total number of integrated reflections 15646
Total number of unique reflections  2952
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   39.4
Average Sigma(I)    1.8
Overall R-merge (linear)  0.121

Sadabs Results

Parameter refinement on 9597 reflections reduced R(int) from 0.2579 to 0.0946

Before rejection, 15717 reflections total and 3000 unique

After rejection, 15274 reflections total and 3000 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.1114   0.643 - 1.745   0.920 - 1.330   1.359    7688    4885
    2   -7.8  0.1597   0.183 - 0.224   0.976 - 1.139   1.502     589     329
    3   -7.8  0.0852   0.671 - 1.376   0.963 - 1.306   1.274    2384    1682
    4   -7.8  0.0867   0.175 - 0.207   0.921 - 1.079   1.253     937     680
    5   -7.8  0.1041   0.663 - 0.853   0.920 - 1.089   1.312    1289     897
    6   -7.8  0.1146   0.787 - 1.024   0.958 - 1.161   1.373    2387    1481
Ratio of minimum to maximum apparent transmission: 0.691843

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp7 d1  
  Formula   C6H8O4N2  
  Crystal Colour    Colourless  
  Crystal Habit    Fragment  
  Crystal Size   0.15 x 0.07 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/