EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2010src0243

Report generated Mar 23, 2010; 08:37:25

Unit cell

34803 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)6.98360 +/- 0.00010
b (Angstrom)12.0495 +/- 0.0002
c (Angstrom)13.2116 +/- 0.0002
alpha (°)90.0137 +/- 0.0009
beta (°)89.9903 +/- 0.0009
gamma (°)88.4684 +/- 0.0010
Volume (A**3)1111.34 +/- 0.03
Mosaicity (°)0.5210 +/- 0.0010

Data collection

Summary

Total number of images collected987
Total exposure time12.4 hours
Data collection exposure time12.3 hours
Data collection wall-clock time13.7 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance39.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f363363.0° phi1.000°45 secondsYes
data collections02f36 36.0° omega1.000°45 secondsYes
data collections03f33 33.0° omega1.000°45 secondsYes
data collections04f61 61.0° omega1.000°45 secondsYes
data collections05f129129.0° omega1.000°45 secondsYes
data collections06f85 85.0° omega1.000°45 secondsYes
data collections07f127127.0° omega1.000°45 secondsYes
data collections08f78 78.0° omega1.000°45 secondsYes
data collections09f67 67.0° omega1.000°45 secondsYes
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected  26
Overload or incomplete profile 756
Sigma cutoff  16
High resolution limit 201

Final Data Set

Scale factor10.00
Number of 'full' reflections  9368
Number of 'partial' reflections 19087
Total number of integrated reflections 24934
Total number of unique reflections  5061
Data completeness  99.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  310.6
Average Sigma(I)    6.5
Overall R-merge (linear)  0.061

Sadabs Results

Estimated minimum and maximum transmission: 0.6746 0.7456

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Prof P.G Taylor  
  Local Code   EY258-CHCl3  
  Formula   C56 H52 F73 N O12 Si8  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Block  
  Crystal Size   0.42 x 0.38 x 0.28 (mm3) 
  Temperature   170(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/