EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2008src0843

Report generated Jul 15, 2008; 17:07:33

Unit cell

55163 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)8.2973 +/- 0.0003
b (Angstrom)13.8488 +/- 0.0005
c (Angstrom)18.2558 +/- 0.0005
alpha (°)98.021 +/- 0.002
beta (°)90.671 +/- 0.002
gamma (°)91.1663 +/- 0.0017
Volume (A**3)2076.55 +/- 0.12
Mosaicity (°)0.986 +/- 0.002

Data collection

Summary

Total number of images collected477
Total exposure time112.4 minutes
Data collection exposure time111.1 minutes
Data collection wall-clock time178.6 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance40.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°14 secondsYes
data collections02f18 36.0° omega2.000°14 secondsYes
data collections03f31 62.0° omega2.000°14 secondsYes
data collections04f16 32.0° omega2.000°14 secondsYes
data collections05f36 72.0° omega2.000°14 secondsYes
data collections06f65130.0° omega2.000°14 secondsYes
data collections07f62124.0° omega2.000°14 secondsYes
data collections08f32 64.0° omega2.000°14 secondsYes
data collections09f28 56.0° omega2.000°14 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected  40
Zero sigma or profile test   2
Overload or incomplete profile1726
Sigma cutoff 170
High resolution limit 597

Final Data Set

Scale factor10.00
Number of 'full' reflections 18087
Number of 'partial' reflections 32052
Total number of integrated reflections 46159
Total number of unique reflections  9404
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   64.3
Average Sigma(I)    2.7
Overall R-merge (linear)  0.132

Sadabs Results

Estimated minimum and maximum transmission: 0.6147 0.7455

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr E McDonald  
  Local Code   CMS-B  
  Formula   C24 H23 N O6  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Block  
  Crystal Size   0.43 x 0.28 x 0.16 (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    'graphite'
_diffrn_measurement_device_type   'Bruker-Nonius Roper 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. (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/