EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2005src0806

Report generated Jun 27, 2005; 13:16:31

Unit cell

10745 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)10.4086 +/- 0.0002
b (Angstrom)12.9227 +/- 0.0003
c (Angstrom)18.7136 +/- 0.0004
alpha (°)83.2031 +/- 0.0010
beta (°)79.3796 +/- 0.0013
gamma (°)76.3612 +/- 0.0013
Volume (A**3)2396.83 +/- 0.09
Mosaicity (°)0.5150 +/- 0.0010

Data collection

Summary

Total number of images collected368
Total exposure time122.7 minutes
Data collection exposure time121.3 minutes
Data collection wall-clock time150.4 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance36.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°20 secondsYes
data collections02f16 32.0° omega2.000°20 secondsYes
data collections03f16 32.0° omega2.000°20 secondsYes
data collections04f60120.0° omega2.000°20 secondsYes
data collections05f28 56.0° omega2.000°20 secondsYes
data collections06f59118.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 243
Zero sigma or profile test   5
Overload or incomplete profile1442
Sigma cutoff  13
High resolution limit 274

Final Data Set

Scale factor range7.67-13.54
Number of 'full' reflections 32517
Number of 'partial' reflections 18425
Total number of integrated reflections 49279
Total number of unique reflections 10918
Data completeness 100.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   33.0
Average Sigma(I)    1.6
Overall R-merge (linear)  0.071

Sadabs Results

Parameter refinement on 34254 reflections reduced R(int) from 0.0920 to 0.0565

Before rejection, 48449 reflections total and 11022 unique

After rejection, 47810 reflections total and 11022 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   12.6  0.0709   0.777 - 1.164   0.959 - 1.181   1.398   24031   17330
    2  -12.3  0.0612   0.649 - 0.732   0.976 - 1.180   1.372    1946    1520
    3  -12.3  0.0643   0.549 - 0.585   0.959 - 1.139   1.344    1934    1474
    4  -12.0  0.0606   0.912 - 1.032   0.959 - 1.261   1.356    8203    6235
    5  -12.0  0.0645   0.754 - 0.915   0.959 - 1.159   1.412    3644    2765
    6  -12.0  0.0612   0.828 - 1.014   0.966 - 1.185   1.334    8052    6186
Ratio of minimum to maximum apparent transmission: 0.760575

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. R. B. Bedford  
  Local Code   MB428  
  Formula   C57 H54 O3 P3 Cl Ru  
  Crystal Colour    Colourless  
  Crystal Habit    Slab  
  Crystal Size   0.1 x 0.09 x 0.04 (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    '10cm confocal mirrors'
_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/