EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)


Summary report for Directory: diska/2005src0806b

Report generated Jun 27, 2005; 15:46:26

Unit cell

11708 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)13.1663 +/- 0.0002
b (Angstrom)13.5696 +/- 0.0002
c (Angstrom)15.5439 +/- 0.0002
alpha (°)102.4235 +/- 0.0007
beta (°)104.1498 +/- 0.0009
gamma (°)92.9015 +/- 0.0009
Volume (A**3)2614.12 +/- 0.07
Mosaicity (°)0.4750 +/- 0.0010

Data collection

Summary

Total number of images collected332
Total exposure time88.6 minutes
Data collection exposure time87.5 minutes
Data collection wall-clock time114.5 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°16 secondsYes
data collections02f17 34.0° omega2.000°16 secondsYes
data collections03f17 34.0° omega2.000°16 secondsYes
data collections04f56112.0° omega2.000°16 secondsYes
data collections05f53106.0° omega2.000°16 secondsYes
Phi/Chii01f - i08f88 seconds

Scalepack Scaling

Deleted observations

Rejected 290
Zero sigma or profile test   6
Overload or incomplete profile1752
Sigma cutoff  22
High resolution limit   9

Final Data Set

Scale factor range8.99-10.76
Number of 'full' reflections 39209
Number of 'partial' reflections 20798
Total number of integrated reflections 57849
Total number of unique reflections 11971
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   84.6
Average Sigma(I)    2.4
Overall R-merge (linear)  0.032

Sadabs Results

Parameter refinement on 47359 reflections reduced R(int) from 0.0502 to 0.0304

Before rejection, 57105 reflections total and 11977 unique

After rejection, 56593 reflections total and 11969 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.0329   1.067 - 1.206   0.967 - 1.087   1.369   32360   27411
    2   -7.8  0.0311   0.641 - 0.685   0.993 - 1.038   1.289    2650    2284
    3   -7.8  0.0295   0.982 - 1.028   0.969 - 1.073   1.305    2674    2296
    4   -7.8  0.0310   0.796 - 0.904   0.967 - 1.062   1.297    9745    8440
    5   -7.8  0.0307   0.714 - 0.803   0.975 - 1.045   1.246    9164    7962
Ratio of minimum to maximum apparent transmission: 0.889861

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. R. B. Bedford  
  Local Code   MB428 (large)  
  Formula   C57 H54 O3 P3 Cl1 Ru1  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Block  
  Crystal Size   0.48 x 0.32 x 0.24 (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 V2.10 (Sheldrick, G.M., 2003)'

_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 95mm 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. (2003). SADABS. Version 2.10. 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/