EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: home/diska/2007src1055

Report generated Aug 03, 2007; 16:34:30

Unit cell

12338 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)5.37320 +/- 0.00010
b (Angstrom)13.4962 +/- 0.0004
c (Angstrom)15.8088 +/- 0.0005
alpha (°)95.3885 +/- 0.0013
beta (°)98.4984 +/- 0.0017
gamma (°)101.2010 +/- 0.0018
Volume (A**3)1103.32 +/- 0.05
Mosaicity (°)0.442 +/- 0.002

Data collection

Summary

Total number of images collected327
Total exposure time44.9 minutes
Data collection exposure time44.2 minutes
Data collection wall-clock time68.3 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance31.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f181362.0° phi2.000°8 secondsYes
data collections02f13 26.0° omega2.000°8 secondsYes
data collections03f52104.0° omega2.000°8 secondsYes
data collections04f24 48.0° omega2.000°8 secondsYes
data collections05f49 98.0° omega2.000°8 secondsYes
Phi/Chii01f - i08f85 seconds

Scalepack Scaling

Deleted observations

Rejected   2
Zero sigma or profile test   1
Overload or incomplete profile 592
Sigma cutoff 198
High resolution limit  78

Final Data Set

Scale factor10.00
Number of 'full' reflections 15000
Number of 'partial' reflections  7121
Total number of integrated reflections 21197
Total number of unique reflections  5008
Data completeness  99.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   40.6
Average Sigma(I)    1.3
Overall R-merge (linear)  0.216

Sadabs Results

Parameter refinement on 15813 reflections reduced R(int) from 0.1450 to 0.0586

Before rejection, 21050 reflections total and 5052 unique

After rejection, 18538 reflections total and 5028 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.7  0.0651   0.830 - 1.248   0.983 - 1.130   2.149   10628    7755
    2   11.1  0.0571   0.510 - 0.610   0.995 - 1.050   2.057     657     509
    3   11.1  0.0482   0.519 - 0.959   0.984 - 1.040   1.949    3052    2474
    4   11.1  0.0528   0.839 - 0.984   0.997 - 1.062   2.062    1350    1039
    5   11.1  0.0543   0.511 - 0.994   0.998 - 1.118   2.055    2851    2138
Ratio of minimum to maximum apparent transmission: 0.870535

Metadata

  Group    Service  
  Operator   Louise Male  
  Sample Owner   Dr John Spencer  
  Local Code   Sami cyclohexanone  
  Formula   C14 H15 N1 O1  
  Crystal Colour    Pale Brown  
  Crystal Habit    Needle  
  Crystal Size   0.85 x 0.08 x 0.06 (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/