EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: home/diska/2005slh0421

Report generated May 08, 2005; 17:08:53

Unit cell

5860 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)9.2600 +/- 0.0003
b (Angstrom)10.4422 +/- 0.0003
c (Angstrom)15.0672 +/- 0.0004
alpha (°)79.2581 +/- 0.0015
beta (°)84.6705 +/- 0.0017
gamma (°)65.4151 +/- 0.0015
Volume (A**3)1301.44 +/- 0.07
Mosaicity (°)0.551 +/- 0.002

Data collection

Summary

Total number of images collected296
Total exposure time195.7 minutes
Data collection exposure time193.0 minutes
Data collection wall-clock time218.9 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f181362.0° phi2.000°40 secondsYes
data collections02f16 32.0° omega2.000°40 secondsYes
data collections03f16 32.0° omega2.000°40 secondsYes
data collections04f22 44.0° omega2.000°40 secondsYes
data collections05f53106.0° omega2.000°40 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected 140
Overload or incomplete profile 734
Sigma cutoff  10

Final Data Set

Scale factor range9.89-18.67
Number of 'full' reflections 16926
Number of 'partial' reflections 11135
Total number of integrated reflections 27063
Total number of unique reflections  5970
Data completeness  99.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   39.5
Average Sigma(I)    1.6
Overall R-merge (linear)  0.061

Sadabs Results

Parameter refinement on 19332 reflections reduced R(int) from 0.1112 to 0.0514

Before rejection, 26574 reflections total and 5959 unique

After rejection, 26223 reflections total and 5958 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0602   1.034 - 1.670   0.953 - 1.150   1.358   16666   12637
    2   -6.8  0.0661   0.487 - 0.544   0.953 - 1.085   1.381    1332     982
    3   -6.8  0.0547   1.010 - 1.117   0.965 - 1.093   1.340    1334    1059
    4   -6.8  0.0690   0.483 - 0.607   0.953 - 1.094   1.387    1925    1427
    5   -6.8  0.0507   0.519 - 0.604   0.953 - 1.111   1.243    4966    3975
Ratio of minimum to maximum apparent transmission: 0.828724

Metadata

  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   CAG 149  
  Formula   C34 H32 N6 O4 P2 S4 Ni1  
  Crystal Colour    Red  
  Crystal Habit    Lath  
  Crystal Size   0.12 x 0.04 x 0.02 (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/