EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2009src0267

Report generated Mar 11, 2009; 13:07:12

Unit cell

57797 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)12.2480 +/- 0.0003
b (Angstrom)9.1264 +/- 0.0003
c (Angstrom)25.8185 +/- 0.0007
alpha (°) 90.000
beta (°)96.5614 +/- 0.0016
gamma (°) 90.000
Volume (A**3)2867.09 +/- 0.14
Mosaicity (°)0.7560 +/- 0.0010

Data collection

Summary

Total number of images collected539
Total exposure time217.9 minutes
Data collection exposure time215.2 minutes
Data collection wall-clock time248.6 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance38.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f92110.4° omega1.200°24 secondsYes
data collections02f97116.4° omega1.200°24 secondsYes
data collections03f97116.4° omega1.200°24 secondsYes
data collections04f98117.6° omega1.200°24 secondsYes
data collections05f81 97.2° omega1.200°24 secondsYes
data collections06f66 79.2° omega1.200°24 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected   5
Zero sigma or profile test  63
Overload or incomplete profile1474
Sigma cutoff1111
High resolution limit 112

Final Data Set

Scale factor10.00
Number of 'full' reflections 10086
Number of 'partial' reflections 35314
Total number of integrated reflections 40055
Total number of unique reflections  6942
Data completeness  99.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   15.1
Average Sigma(I)    1.0
Overall R-merge (linear)  0.195

Sadabs Results

Parameter refinement on 25049 reflections reduced R(int) from 0.1441 to 0.0697

Before rejection, 43064 reflections total and 7007 unique

After rejection, 36613 reflections total and 6983 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    6.6  0.0884   0.669 - 1.393   0.973 - 1.450   1.997    6082    3677
    2   14.2  0.0863   0.830 - 1.319   0.954 - 1.350   1.955    6807    3902
    3   16.9  0.1135   0.476 - 0.624   0.973 - 1.370   2.100    6814    3443
    4   16.9  0.1063   0.705 - 0.948   0.955 - 1.395   2.051    6862    3634
    5   16.9  0.0988   0.851 - 0.973   0.964 - 1.144   2.046    5553    2882
    6   16.9  0.1068   0.853 - 1.120   0.956 - 1.501   2.081    4495    2296
Ratio of minimum to maximum apparent transmission: 0.635709

Metadata

  Group    Service  
  Operator   Sam Callear  
  Sample Owner   Dr J Spencer  
  Local Code   sp02  
  Formula   C25H45B2F4O2P  
  Crystal Colour    Colourless  
  Crystal Habit    Lath  
  Crystal Size   0.21 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/