EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007src0217

Report generated Feb 14, 2007; 16:04:56

Unit cell

2878 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)8.7987 +/- 0.0003
b (Angstrom)9.0106 +/- 0.0002
c (Angstrom)9.3873 +/- 0.0003
alpha (°)73.958 +/- 0.002
beta (°)78.1009 +/- 0.0016
gamma (°)63.8458 +/- 0.0018
Volume (A**3)638.94 +/- 0.03
Mosaicity (°)0.577 +/- 0.002

Data collection

Summary

Total number of images collected342
Total exposure time103.4 minutes
Data collection exposure time102.0 minutes
Data collection wall-clock time163.3 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°18 secondsYes
data collections02f13 26.0° omega2.000°18 secondsYes
data collections03f13 26.0° omega2.000°18 secondsYes
data collections04f52104.0° omega2.000°18 secondsYes
data collections05f26 52.0° omega2.000°18 secondsYes
data collections06f49 98.0° omega2.000°18 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 301
Overload or incomplete profile 480
Sigma cutoff  64

Final Data Set

Scale factor range8.18-14.57
Number of 'full' reflections  7765
Number of 'partial' reflections  5510
Total number of integrated reflections 12572
Total number of unique reflections  2937
Data completeness  99.4%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  183.3
Average Sigma(I)    3.6
Overall R-merge (linear)  0.043

Sadabs Results

Parameter refinement on 11082 reflections reduced R(int) from 0.1327 to 0.0361

Before rejection, 12694 reflections total and 2945 unique

After rejection, 11719 reflections total and 2941 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.7  0.0385   0.690 - 1.403   0.988 - 1.066   2.344    6474    5635
    2   11.1  0.0307   0.778 - 0.838   0.991 - 1.046   2.158     401     347
    3   11.1  0.0365   0.492 - 0.546   0.989 - 1.047   2.275     396     345
    4   11.1  0.0311   0.752 - 1.167   0.987 - 1.025   2.203    1841    1629
    5   11.1  0.0327   0.528 - 0.651   0.989 - 1.052   2.139     877     765
    6   11.1  0.0304   0.701 - 1.005   0.988 - 1.056   2.193    1730    1510
Ratio of minimum to maximum apparent transmission: 0.925823

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. M. A. Beckett  
  Local Code   MAB/DK9 BANGOR  
  Formula   C7 H20 N1 O11 B5  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.22 x 0.17 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    '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/