EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2008lsh009

Report generated Jun 21, 2008; 15:00:58

Unit cell

13033 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)5.0214 +/- 0.0003
b (Angstrom)6.8411 +/- 0.0005
c (Angstrom)12.2219 +/- 0.0010
alpha (°)89.465 +/- 0.004
beta (°)80.477 +/- 0.005
gamma (°)79.234 +/- 0.004
Volume (A**3)406.67 +/- 0.05
Mosaicity (°)1.265 +/- 0.004

Data collection

Summary

Total number of images collected328
Total exposure time216.4 minutes
Data collection exposure time215.0 minutes
Data collection wall-clock time233.9 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 collections01f51102.0° omega2.000°40 secondsYes
data collections02f48 96.0° omega2.000°40 secondsYes
data collections03f49 98.0° omega2.000°40 secondsYes
data collections04f51102.0° omega2.000°40 secondsYes
data collections05f23 46.0° omega2.000°40 secondsYes
data collections06f50100.0° omega2.000°40 secondsYes
data collections07f48 96.0° omega2.000°40 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected   1
Zero sigma or profile test   1
Overload or incomplete profile 258
Sigma cutoff 198
High resolution limit  33

Final Data Set

Scale factor10.00
Number of 'full' reflections  1755
Number of 'partial' reflections  6984
Total number of integrated reflections  7749
Total number of unique reflections  1849
Data completeness  99.6%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   87.8
Average Sigma(I)    2.8
Overall R-merge (linear)  0.223

Sadabs Results

Parameter refinement on 5790 reflections reduced R(int) from 0.1481 to 0.0532

Before rejection, 7989 reflections total and 1866 unique

After rejection, 6987 reflections total and 1855 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.4  0.0542   0.709 - 1.125   0.902 - 1.097   1.953    1128     846
    2   10.2  0.0528   1.693 - 2.825   0.969 - 1.097   2.124    1081     745
    3   10.2  0.0576   0.689 - 0.994   0.968 - 1.123   2.029    1083     811
    4   10.2  0.0547   0.546 - 0.856   0.923 - 1.097   2.003    1095     833
    5   10.2  0.0712   0.291 - 0.336   1.005 - 1.122   2.164     456     288
    6   10.2  0.0595   1.832 - 2.863   0.970 - 1.124   2.109    1114     812
    7   10.2  0.0660   0.520 - 0.871   0.922 - 1.123   2.134    1030     712
Ratio of minimum to maximum apparent transmission: 0.802876

Metadata

  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   PAA/COOH  
  Formula   C9 H9 N1 O3  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.12 x 0.08 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 2007/2 (Sheldrick, G.M., 2007)'

_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 APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

_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. (2007). SADABS. Version 2007/2. 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/