EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007src0218r

Report generated Feb 16, 2007; 13:28:50

Unit cell

3593 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)9.3242 +/- 0.0002
b (Angstrom)9.3250 +/- 0.0002
c (Angstrom)9.8196 +/- 0.0003
alpha (°)79.0779 +/- 0.0014
beta (°)79.0573 +/- 0.0013
gamma (°)75.8330 +/- 0.0017
Volume (A**3)803.55 +/- 0.04
Mosaicity (°)0.6020 +/- 0.0010

Data collection

Summary

Total number of images collected722
Total exposure time148.0 minutes
Data collection exposure time146.6 minutes
Data collection wall-clock time179.1 minutes

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 collections01f363363.0° phi1.000°12 secondsYes
data collections02f26 26.0° omega1.000°12 secondsYes
data collections03f56 56.0° omega1.000°12 secondsYes
data collections04f55 55.0° omega1.000°12 secondsYes
data collections05f111111.0° omega1.000°12 secondsYes
data collections06f103103.0° omega1.000°12 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 432
Zero sigma or profile test  10
Overload or incomplete profile 584
Sigma cutoff 118
High resolution limit  18

Final Data Set

Scale factor range6.75-13.55
Number of 'full' reflections  3685
Number of 'partial' reflections 11587
Total number of integrated reflections 14505
Total number of unique reflections  3671
Data completeness  99.3%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  122.8
Average Sigma(I)    2.7
Overall R-merge (linear)  0.048

Sadabs Results

Parameter refinement on 11787 reflections reduced R(int) from 0.1703 to 0.0383

Before rejection, 14919 reflections total and 3701 unique

After rejection, 13485 reflections total and 3688 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.1  0.0407   0.688 - 1.507   0.964 - 1.054   2.143    6882    5414
    2   14.6  0.0374   0.331 - 0.365   0.978 - 1.053   2.113     468     366
    3   14.6  0.0359   0.667 - 0.904   0.990 - 1.085   2.197    1045     763
    4   14.6  0.0389   1.715 - 2.275   0.978 - 1.076   2.184    1005     761
    5   14.6  0.0384   0.609 - 1.065   0.967 - 1.082   2.082    2131    1682
    6   14.6  0.0367   0.730 - 0.867   0.964 - 1.079   2.003    1954    1612
Ratio of minimum to maximum apparent transmission: 0.888353

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. M. A. Beckett  
  Local Code   MAB/DK8  
  Formula   C4 H14 N1 O11 B5  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.22 x 0.2 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/