EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2009src1289

Report generated Nov 27, 2009; 16:44:59

Unit cell

10388 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)8.9198 +/- 0.0003
b (Angstrom)8.9196 +/- 0.0002
c (Angstrom)9.7074 +/- 0.0003
alpha (°)107.7514 +/- 0.0017
beta (°)110.1653 +/- 0.0012
gamma (°)91.7154 +/- 0.0017
Volume (A**3)682.55 +/- 0.04
Mosaicity (°)0.565 +/- 0.002

Data collection

Summary

Total number of images collected315
Total exposure time105.3 minutes
Data collection exposure time104.0 minutes
Data collection wall-clock time117.1 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°20 secondsYes
data collections02f13 26.0° omega2.000°20 secondsYes
data collections03f13 26.0° omega2.000°20 secondsYes
data collections04f24 48.0° omega2.000°20 secondsYes
data collections05f24 48.0° omega2.000°20 secondsYes
data collections06f52104.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Zero sigma or profile test   3
Overload or incomplete profile 342
Sigma cutoff  46

Final Data Set

Scale factor10.00
Number of 'full' reflections  7893
Number of 'partial' reflections  5364
Total number of integrated reflections 12635
Total number of unique reflections  3145
Data completeness  99.6%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  460.2
Average Sigma(I)    9.3
Overall R-merge (linear)  0.104

Sadabs Results

Parameter refinement on 11532 reflections reduced R(int) from 0.0808 to 0.0335

Before rejection, 12397 reflections total and 3141 unique

After rejection, 11764 reflections total and 3133 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.7  0.0359   0.843 - 1.152   0.943 - 1.164   2.519    7093    6580
    2   11.1  0.0335   0.700 - 0.865   0.952 - 1.138   2.356     440     403
    3   11.1  0.0291   0.739 - 0.820   0.948 - 1.125   2.218     432     399
    4   11.1  0.0268   0.818 - 0.955   0.959 - 1.136   2.299     897     848
    5   11.1  0.0264   0.908 - 0.973   0.958 - 1.124   2.307     883     835
    6   11.1  0.0301   0.808 - 1.269   0.943 - 1.097   2.367    2019    1887
Ratio of minimum to maximum apparent transmission: 0.810096

Metadata

  Group    Service  
  Operator   Graham Tizzard  
  Sample Owner   Dr A Fogg  
  Local Code   JN434  
  Formula   Nd2C6H17O16P3  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.06 x 0.05 x 0.01 (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/