EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)


Summary report for Directory: diska/2007src0546

Report generated Apr 20, 2007; 15:20:17

Unit cell

6753 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)9.58220 +/- 0.00010
b (Angstrom)16.9680 +/- 0.0005
c (Angstrom)18.0459 +/- 0.0005
alpha (°) 90.000
beta (°)97.1977 +/- 0.0016
gamma (°) 90.000
Volume (A**3)2910.98 +/- 0.12
Mosaicity (°)0.4280 +/- 0.0010

Data collection

Summary

Total number of images collected208
Total exposure time68.5 minutes
Data collection exposure time67.4 minutes
Data collection wall-clock time94.9 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f166332.0° phi2.000°20 secondsYes
data collections02f17 34.0° omega2.000°20 secondsYes
data collections03f17 34.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f88 seconds

Scalepack Scaling

Deleted observations

Rejected 204
Zero sigma or profile test   2
Overload or incomplete profile1086
Sigma cutoff 160
High resolution limit   2

Final Data Set

Scale factor range9.79-10.93
Number of 'full' reflections 29741
Number of 'partial' reflections 13262
Total number of integrated reflections 40565
Total number of unique reflections  6903
Data completeness  99.5%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   50.4
Average Sigma(I)    1.8
Overall R-merge (linear)  0.055

Sadabs Results

Parameter refinement on 24939 reflections reduced R(int) from 0.0738 to 0.0429

Before rejection, 41278 reflections total and 6905 unique

After rejection, 40743 reflections total and 6901 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0559   0.926 - 1.015   0.938 - 1.132   1.323   34310   22066
    2   -6.8  0.0559   0.708 - 0.759   0.937 - 1.126   1.303    3220    2121
    3   -6.8  0.0559   0.674 - 0.734   0.935 - 1.132   1.298    3213    2074
Ratio of minimum to maximum apparent transmission: 0.825683

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Tomkinson  
  Local Code   TG 3.145  
  Formula   C13H16NPF6  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.2 x 0.12 x 0.04 (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 V2.10 (Sheldrick, G.M., 2003)'

_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 95mm 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. (2003). SADABS. Version 2.10. 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/