EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)


Summary report for Directory: diska/2009src1142

Report generated Oct 23, 2009; 14:05:00

Unit cell

40505 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)12.0419 +/- 0.0010
b (Angstrom)5.7992 +/- 0.0006
c (Angstrom)20.795 +/- 0.002
alpha (°) 90.000
beta (°)89.999 +/- 0.006
gamma (°) 90.000
Volume (A**3)1452.2 +/- 0.2
Mosaicity (°)1.940 +/- 0.004

Data collection

Summary

Total number of images collected275
Total exposure time73.5 minutes
Data collection exposure time72.1 minutes
Data collection wall-clock time94.4 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance32.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f154246.4° phi1.600°16 secondsYes
data collections02f21 33.6° omega1.600°16 secondsYes
data collections03f20 32.0° omega1.600°16 secondsYes
data collections04f72115.2° omega1.600°16 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected  32
Zero sigma or profile test  26
Overload or incomplete profile 840
Sigma cutoff  31
High resolution limit  33

Final Data Set

Scale factor10.00
Number of 'full' reflections     0
Number of 'partial' reflections 16400
Total number of integrated reflections 12489
Total number of unique reflections  3161
Data completeness  86.3%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   27.9
Average Sigma(I)    2.3
Overall R-merge (linear)  0.159

Sadabs Results

Estimated minimum and maximum transmission: 0.5074 0.7456

Metadata

  Group    Service  
  Operator   Graham Tizzard  
  Sample Owner   Dr I Collins  
  Local Code   AJW-1546-46  
  Formula   C17H24O3  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.4 x 0.2 x 0.03 (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/