EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2008src0009

Report generated Jan 10, 2008; 17:44:03

Unit cell

14310 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p2
a (Angstrom)18.3051 +/- 0.0005
b (Angstrom)8.13900 +/- 0.00010
c (Angstrom)39.2691 +/- 0.0009
alpha (°) 90.000
beta (°)101.6625 +/- 0.0010
gamma (°) 90.000
Volume (A**3)5729.7 +/- 0.2
Mosaicity (°)0.2830 +/- 0.0010

Data collection

Summary

Total number of images collected315
Total exposure time104.8 minutes
Data collection exposure time103.5 minutes
Data collection wall-clock time130.8 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance46.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f152304.0° phi2.000°20 secondsYes
data collections02f17 34.0° omega2.000°20 secondsYes
data collections03f69138.0° omega2.000°20 secondsYes
data collections04f69138.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected  55
Zero sigma or profile test  27
Overload or incomplete profile1076
Sigma cutoff 104
High resolution limit 294

Final Data Set

Scale factor10.00
Number of 'full' reflections 41842
Number of 'partial' reflections 10195
Total number of integrated reflections 49547
Total number of unique reflections 12166
Data completeness  87.1%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   18.4
Average Sigma(I)    1.4
Overall R-merge (linear)  0.107

Sadabs Results

Estimated minimum and maximum transmission: 0.6551 0.7456

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Prof DB Davies  
  Local Code   307-478-B  
  Formula   C5H13Cl3N5OP3  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.28 x 0.2 x 0.05 (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    'graphite'
_diffrn_measurement_device_type   'Bruker-Nonius Roper 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. (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/