EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2009src0216r

Report generated Mar 02, 2009; 18:05:44

Unit cell

16828 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)6.2066 +/- 0.0003
b (Angstrom)17.1960 +/- 0.0008
c (Angstrom)15.1712 +/- 0.0006
alpha (°) 90.000
beta (°)90.442 +/- 0.003
gamma (°) 90.000
Volume (A**3)1619.15 +/- 0.13
Mosaicity (°)0.626 +/- 0.002

Data collection

Summary

Total number of images collected251
Total exposure time149.1 minutes
Data collection exposure time147.1 minutes
Data collection wall-clock time160.1 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance32.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f123246.0° phi2.000°36 secondsYes
data collections02f13 26.0° omega2.000°36 secondsYes
data collections03f25 50.0° omega2.000°36 secondsYes
data collections04f31 62.0° omega2.000°36 secondsYes
data collections05f51102.0° omega2.000°36 secondsYes
Phi/Chii01f - i08f815 seconds

Scalepack Scaling

Deleted observations

Rejected   5
Zero sigma or profile test   7
Overload or incomplete profile 500
Sigma cutoff 446
High resolution limit  72

Final Data Set

Scale factor10.00
Number of 'full' reflections 13323
Number of 'partial' reflections 10606
Total number of integrated reflections 22406
Total number of unique reflections  3822
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   13.1
Average Sigma(I)    0.9
Overall R-merge (linear)  0.206

Sadabs Results

Parameter refinement on 13981 reflections reduced R(int) from 0.1354 to 0.0937

Before rejection, 22341 reflections total and 3847 unique

After rejection, 18947 reflections total and 3828 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   12.6  0.1294   0.724 - 0.900   0.967 - 1.222   2.045    9819    5620
    2   12.0  0.1308   0.583 - 0.608   0.967 - 1.098   2.049     899     520
    3   12.0  0.1197   0.750 - 0.849   1.014 - 1.159   2.049    1899    1128
    4   12.0  0.1195   0.732 - 0.886   0.987 - 1.152   1.990    2373    1450
    5   12.0  0.1183   0.756 - 0.943   1.014 - 1.215   1.962    3957    2374
Ratio of minimum to maximum apparent transmission: 0.791249

Metadata

  Group    Service  
  Operator   Sam Callear  
  Sample Owner   Dr J Spencer  
  Local Code   RRPSAN02  
  Formula   C14H21ClN3PPdS  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.09 x 0.07 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/