EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2008src0817

Report generated Jul 08, 2008; 14:19:15

Unit cell

4629 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)5.7619 +/- 0.0002
b (Angstrom)6.3796 +/- 0.0002
c (Angstrom)11.6206 +/- 0.0005
alpha (°)92.684 +/- 0.002
beta (°)98.060 +/- 0.002
gamma (°)114.750 +/- 0.002
Volume (A**3)381.43 +/- 0.03
Mosaicity (°)0.449 +/- 0.002

Data collection

Summary

Total number of images collected361
Total exposure time97.4 minutes
Data collection exposure time96.0 minutes
Data collection wall-clock time116.3 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 collections01f126252.0° phi2.000°16 secondsYes
data collections02f52104.0° omega2.000°16 secondsYes
data collections03f47 94.0° omega2.000°16 secondsYes
data collections04f52104.0° omega2.000°16 secondsYes
data collections05f24 48.0° omega2.000°16 secondsYes
data collections06f52104.0° omega2.000°16 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected   1
Zero sigma or profile test   1
Overload or incomplete profile 204
Sigma cutoff  50
High resolution limit  11

Final Data Set

Scale factor10.00
Number of 'full' reflections  5500
Number of 'partial' reflections  2677
Total number of integrated reflections  7548
Total number of unique reflections  1761
Data completeness  99.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  120.0
Average Sigma(I)    2.7
Overall R-merge (linear)  0.136

Sadabs Results

Parameter refinement on 6828 reflections reduced R(int) from 0.1092 to 0.0466

Before rejection, 8163 reflections total and 1773 unique

After rejection, 7332 reflections total and 1764 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.7  0.0560   0.702 - 1.117   0.969 - 1.106   2.217    2571    2107
    2   11.1  0.0425   0.922 - 1.317   0.969 - 1.060   2.245    1098     904
    3   11.1  0.0353   0.572 - 0.907   0.986 - 1.117   2.030     983     845
    4   11.1  0.0355   0.697 - 1.194   0.969 - 1.046   2.087    1093     928
    5   11.1  0.0397   0.723 - 0.891   0.984 - 1.049   2.103     480     423
    6   11.1  0.0344   0.866 - 1.066   0.982 - 1.100   2.098    1107     946
Ratio of minimum to maximum apparent transmission: 0.867421

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr MA Beckett  
  Local Code   MAB/JT/11  
  Formula   C4 H15 N2 O10 B5  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Block  
  Crystal Size   0.08 x 0.05 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 2007/2 (Sheldrick, G.M., 2007)'

_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 APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

_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. (2007). SADABS. Version 2007/2. 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/