EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/07skc0014

Report generated Feb 17, 2007; 14:09:47

Unit cell

2815 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)6.7455 +/- 0.0004
b (Angstrom)8.7156 +/- 0.0005
c (Angstrom)11.3064 +/- 0.0006
alpha (°)101.835 +/- 0.003
beta (°)91.511 +/- 0.003
gamma (°)92.365 +/- 0.003
Volume (A**3)649.62 +/- 0.06
Mosaicity (°)0.479 +/- 0.003

Data collection

Summary

Total number of images collected314
Total exposure time105.0 minutes
Data collection exposure time103.6 minutes
Data collection wall-clock time119.1 minutes

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 collections01f181362.0° phi2.000°20 secondsYes
data collections02f28 56.0° omega2.000°20 secondsYes
data collections03f13 26.0° omega2.000°20 secondsYes
data collections04f28 56.0° omega2.000°20 secondsYes
data collections05f28 56.0° omega2.000°20 secondsYes
data collections06f28 56.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 297
Zero sigma or profile test   2
Overload or incomplete profile 286
Sigma cutoff  86
High resolution limit  47

Final Data Set

Scale factor range7.58-12.72
Number of 'full' reflections  6634
Number of 'partial' reflections  3501
Total number of integrated reflections  9633
Total number of unique reflections  2948
Data completeness  98.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   31.3
Average Sigma(I)    1.3
Overall R-merge (linear)  0.079

Sadabs Results

Parameter refinement on 6962 reflections reduced R(int) from 0.1939 to 0.0539

Before rejection, 9851 reflections total and 2998 unique

After rejection, 8728 reflections total and 2970 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.9  0.0572   0.812 - 1.809   0.945 - 1.082   2.039    5255    3737
    2   15.4  0.0519   0.842 - 1.092   0.944 - 1.051   2.018     793     570
    3   15.4  0.0615   0.141 - 0.151   0.999 - 1.061   2.008     333     252
    4   15.4  0.0574   0.731 - 0.863   0.994 - 1.061   2.044     781     567
    5   15.4  0.0584   0.714 - 0.913   0.950 - 1.034   2.052     791     555
    6   15.4  0.0622   0.392 - 0.485   0.994 - 1.062   2.076     775     534
Ratio of minimum to maximum apparent transmission: 0.871863

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp11 f9  
  Formula   C10H11O4N1  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.16 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/