EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2005src0721

Report generated Jun 15, 2005; 07:39:08

Unit cell

9641 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)12.4468 +/- 0.0009
b (Angstrom)14.3866 +/- 0.0013
c (Angstrom)14.4127 +/- 0.0011
alpha (°)61.994 +/- 0.003
beta (°)84.131 +/- 0.005
gamma (°)88.819 +/- 0.005
Volume (A**3)2265.6 +/- 0.3
Mosaicity (°)2.280 +/- 0.003

Data collection

Summary

Total number of images collected361
Total exposure time15.8 hours
Data collection exposure time15.7 hours
Data collection wall-clock time16.4 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance35.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°160 secondsYes
data collections02f16 32.0° omega2.000°160 secondsYes
data collections03f16 32.0° omega2.000°160 secondsYes
data collections04f27 54.0° omega2.000°160 secondsYes
data collections05f27 54.0° omega2.000°160 secondsYes
data collections06f27 54.0° omega2.000°160 secondsYes
data collections07f59118.0° omega2.000°160 secondsYes
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected 480
Zero sigma or profile test   6
Overload or incomplete profile2944
Sigma cutoff 220
High resolution limit 175

Final Data Set

Scale factor range5.38-11.13
Number of 'full' reflections     0
Number of 'partial' reflections 47955
Total number of integrated reflections 41939
Total number of unique reflections 10238
Data completeness  97.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   36.7
Average Sigma(I)    3.4
Overall R-merge (linear)  0.123

Sadabs Results

Parameter refinement on 20654 reflections reduced R(int) from 0.1130 to 0.0738

Before rejection, 44171 reflections total and 10447 unique

After rejection, 43061 reflections total and 10441 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0899   0.882 - 1.212   0.873 - 1.471   1.330   22900   13379
    2  -11.2  0.1182   0.563 - 0.618   0.929 - 1.534   1.397    1641     885
    3  -10.9  0.1271   0.427 - 0.465   0.928 - 1.152   1.338    1694     934
    4  -11.2  0.1613   0.595 - 0.659   0.918 - 1.562   1.501    3200    1527
    5  -11.2  0.1843   0.595 - 0.696   0.874 - 1.266   1.529    3081    1265
    6  -11.2  0.2219   0.510 - 0.611   0.947 - 1.246   1.588    3094    1150
    7  -11.2  0.1621   0.885 - 1.276   0.919 - 1.266   1.470    7451    3483
Ratio of minimum to maximum apparent transmission: 0.558991

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. S. J. Lancaster  
  Local Code   AM539  
  Formula   C44 H18 B2 F30 Li1 O4 P1  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Blade  
  Crystal Size   0.14 x 0.05 x 0.02 (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/