EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/04skc0011

Report generated Dec 10, 2004; 16:43:14

Unit cell

13192 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)13.9431 +/- 0.0003
b (Angstrom)14.3234 +/- 0.0002
c (Angstrom)16.4841 +/- 0.0003
alpha (°)64.3287 +/- 0.0011
beta (°)78.7517 +/- 0.0009
gamma (°)89.7051 +/- 0.0012
Volume (A**3)2898.39 +/- 0.10
Mosaicity (°)0.4580 +/- 0.0010

Data collection

Summary

Total number of images collected358
Total exposure time119.3 minutes
Data collection exposure time117.9 minutes
Data collection wall-clock time146.4 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 collections01f181362.0° phi2.000°20 secondsYes
data collections02f16 32.0° omega2.000°20 secondsYes
data collections03f16 32.0° omega2.000°20 secondsYes
data collections04f56112.0° omega2.000°20 secondsYes
data collections05f25 50.0° omega2.000°20 secondsYes
data collections06f56112.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 163
Zero sigma or profile test   1
Overload or incomplete profile2346
Sigma cutoff  33
High resolution limit  23

Final Data Set

Scale factor range4.65-10.80
Number of 'full' reflections 46863
Number of 'partial' reflections 23139
Total number of integrated reflections 67972
Total number of unique reflections 13348
Data completeness  99.5%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   38.5
Average Sigma(I)    2.0
Overall R-merge (linear)  0.080

Sadabs Results

Parameter refinement on 41065 reflections reduced R(int) from 0.1147 to 0.0571

Before rejection, 65965 reflections total and 13357 unique

After rejection, 65173 reflections total and 13357 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.3  0.0731   1.042 - 1.671   0.961 - 1.131   1.403   33759   22496
    2   -8.7  0.0740   0.754 - 0.858   0.961 - 1.141   1.404    2727    1826
    3   -8.7  0.0704   0.566 - 0.608   0.961 - 1.098   1.387    2739    1893
    4   -8.7  0.0698   0.414 - 0.511   0.961 - 1.103   1.387   10695    7313
    5   -8.7  0.1152   0.944 - 1.338   0.969 - 1.095   1.512    4536    2566
    6   -8.7  0.0779   1.151 - 1.279   0.961 - 1.158   1.397   10717    6815
Ratio of minimum to maximum apparent transmission: 0.829863

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear (skc)  
  Sample Owner     
  Local Code   TLT374C EF34  
  Formula   C12H30N4O6Br1  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.1 x 0.08 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 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    '10cm confocal mirrors'
_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/