EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2008src0845

Report generated Jul 15, 2008; 14:31:12

Unit cell

81381 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p2
a (Angstrom)21.5955 +/- 0.0007
b (Angstrom)9.5241 +/- 0.0003
c (Angstrom)30.6167 +/- 0.0010
alpha (°) 90.000
beta (°)107.4309 +/- 0.0010
gamma (°) 90.000
Volume (A**3)6008.0 +/- 0.3
Mosaicity (°)0.6690 +/- 0.0010

Data collection

Summary

Total number of images collected580
Total exposure time147.4 minutes
Data collection exposure time146.1 minutes
Data collection wall-clock time181.8 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance50.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f297297.0° phi1.000°15 secondsYes
data collections02f136136.0° omega1.000°15 secondsYes
data collections03f139139.0° omega1.000°15 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected   2
Zero sigma or profile test  47
Overload or incomplete profile1154
Sigma cutoff1406
High resolution limit  40

Final Data Set

Scale factor10.00
Number of 'full' reflections 14013
Number of 'partial' reflections 50513
Total number of integrated reflections 57712
Total number of unique reflections 14499
Data completeness  99.5%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   50.2
Average Sigma(I)    1.7
Overall R-merge (linear)  0.127

Sadabs Results

Parameter refinement on 36537 reflections reduced R(int) from 0.0801 to 0.0430

Before rejection, 62717 reflections total and 14584 unique

After rejection, 53794 reflections total and 14524 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   24.7  0.0556   0.734 - 0.968   0.983 - 1.057   2.095   27755   15207
    2   24.1  0.0453   0.857 - 1.243   0.993 - 1.049   1.988   12871    7757
    3   24.1  0.0511   0.822 - 0.979   0.988 - 1.051   2.070   13168    7182
Ratio of minimum to maximum apparent transmission: 0.929860

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr E McDonald  
  Local Code   CMS-F  
  Formula   C23 H20 N2 O6  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Block  
  Crystal Size   0.16 x 0.13 x 0.09 (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/