EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/07skc0017

Report generated Feb 18, 2007; 07:29:22

Unit cell

873 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)5.0677 +/- 0.0003
b (Angstrom)5.5919 +/- 0.0004
c (Angstrom)7.2474 +/- 0.0004
alpha (°)91.982 +/- 0.003
beta (°)103.964 +/- 0.004
gamma (°)99.506 +/- 0.003
Volume (A**3)195.98 +/- 0.02
Mosaicity (°)0.519 +/- 0.003

Data collection

Summary

Total number of images collected356
Total exposure time10.8 hours
Data collection exposure time10.7 hours
Data collection wall-clock time10.9 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance36.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f146292.0° phi2.000°110 secondsYes
data collections02f28 56.0° omega2.000°110 secondsYes
data collections03f56112.0° omega2.000°110 secondsYes
data collections04f34 68.0° omega2.000°110 secondsYes
data collections05f56112.0° omega2.000°110 secondsYes
data collections06f28 56.0° omega2.000°110 secondsYes
Phi/Chii01f - i08f860 seconds

Scalepack Scaling

Deleted observations

Rejected  84
Zero sigma or profile test   2
Overload or incomplete profile 144
Sigma cutoff  13
Low resolution limit   4
High resolution limit  17

Final Data Set

Scale factor range10.00-15.35
Number of 'full' reflections  2233
Number of 'partial' reflections  1283
Total number of integrated reflections  3301
Total number of unique reflections   893
Data completeness  99.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  362.4
Average Sigma(I)    7.3
Overall R-merge (linear)  0.055

Sadabs Results

Parameter refinement on 3009 reflections reduced R(int) from 0.1042 to 0.0458

Before rejection, 3369 reflections total and 907 unique

After rejection, 3187 reflections total and 903 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.9  0.0476   0.932 - 1.716   0.962 - 1.050   2.139    1331    1195
    2   15.4  0.0559   0.973 - 1.080   0.970 - 1.048   2.201     255     230
    3   15.4  0.0431   0.687 - 0.842   0.970 - 1.046   2.117     513     462
    4   15.4  0.0405   0.488 - 0.553   0.971 - 1.047   2.085     312     288
    5   15.4  0.0432   0.757 - 0.957   0.975 - 1.049   2.197     518     463
    6   15.4  0.0424   0.891 - 0.970   0.962 - 1.044   2.061     258     232
Ratio of minimum to maximum apparent transmission: 0.915811

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp11 b9  
  Formula   C6H12O4N2  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.08 x 0.07 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 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/