EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2005src1310

Report generated Oct 28, 2005; 14:26:54

Unit cell

15794 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)17.9696 +/- 0.0013
b (Angstrom)20.8264 +/- 0.0011
c (Angstrom)20.8568 +/- 0.0015
alpha (°)69.203 +/- 0.003
beta (°)83.485 +/- 0.002
gamma (°)83.540 +/- 0.003
Volume (A**3)7227.8 +/- 0.8
Mosaicity (°)1.881 +/- 0.002

Data collection

Summary

Total number of images collected352
Total exposure time117.0 minutes
Data collection exposure time115.9 minutes
Data collection wall-clock time146.7 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance50.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f70140.0° omega2.000°20 secondsYes
data collections02f75150.0° omega2.000°20 secondsYes
data collections03f54108.0° omega2.000°20 secondsYes
data collections04f73146.0° omega2.000°20 secondsYes
data collections05f72144.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f88 seconds

Scalepack Scaling

Deleted observations

Rejected 309
Zero sigma or profile test  33
Overload or incomplete profile5414
Sigma cutoff 164
High resolution limit  97

Final Data Set

Scale factor range8.33-12.41
Number of 'full' reflections  1439
Number of 'partial' reflections 89551
Total number of integrated reflections 63294
Total number of unique reflections 24742
Data completeness  74.4%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   59.2
Average Sigma(I)    4.4
Overall R-merge (linear)  0.054

Sadabs Results

Parameter refinement on 44813 reflections reduced R(int) from 0.0980 to 0.0475

Before rejection, 86663 reflections total and 30310 unique

After rejection, 85014 reflections total and 30283 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1  -10.6  0.0584   0.995 - 1.166   0.967 - 1.354   1.485   15766   10602
    2  -21.1  0.0702   0.854 - 1.013   0.967 - 1.099   1.444   19450   10775
    3   21.1  0.0670   0.690 - 0.869   0.940 - 1.223   1.456   12759    7284
    4  -21.1  0.0698   0.618 - 0.825   0.954 - 1.044   1.447   18892   10907
    5   21.1  0.0706   0.987 - 1.300   0.949 - 1.094   1.477   18147    9737

Sadabs Results

Parameter refinement on 39862 reflections reduced R(int) from 0.0649 to 0.0438

Before rejection, 81877 reflections total and 28905 unique

After rejection, 80859 reflections total and 28904 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   10.6  0.0572   0.851 - 1.000   0.947 - 1.229   1.500   14842    9621
    2   21.1  0.0680   0.819 - 0.988   0.920 - 1.124   1.439   18191    9599
    3  -21.1  0.0762   0.830 - 1.064   0.947 - 1.171   1.478   13046    6530
    4   21.1  0.0720   0.729 - 0.953   0.920 - 1.154   1.486   17183    9356
    5  -21.1  0.0747   0.890 - 1.180   0.920 - 1.102   1.512   17597    8508
Ratio of minimum to maximum apparent transmission: 0.694052

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. S. S. Turner  
  Local Code   PM004  
  Formula   C38 H22 N10 S4 Co1 Ni1  
  Crystal Colour   Opaque Dark Red  
  Crystal Habit    Slab  
  Crystal Size   0.2 x 0.16 x 0.08 (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/