EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/04mbh0607

Report generated Jun 20, 2004; 08:38:51

Unit cell

5055 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
a (Angstrom)7.40620 +/- 0.00010
b (Angstrom)14.2710 +/- 0.0005
c (Angstrom)21.7881 +/- 0.0009
alpha (°) 90.000
beta (°)93.906 +/- 0.002
gamma (°) 90.000
Volume (A**3)2297.52 +/- 0.13
Mosaicity (°)0.352 +/- 0.002

Data collection


Total number of images collected204
Total exposure time8.2 hours
Data collection exposure time8.2 hours
Data collection wall-clock time8.7 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f174261.0° phi1.500°150 secondsYes
data collections02f22 33.0° omega1.500°150 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected 109
Zero sigma or profile test   5
Overload or incomplete profile 644
Sigma cutoff  17
High resolution limit   4

Final Data Set

Scale factor range6.31-10.02
Number of 'full' reflections 16532
Number of 'partial' reflections  8470
Total number of integrated reflections 24404
Total number of unique reflections  5483
Data completeness  99.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   19.9
Average Sigma(I)    1.4
Overall R-merge (linear)  0.065

Sadabs Results

Parameter refinement on 13077 reflections reduced R(int) from 0.0673 to 0.0396

Before rejection, 24187 reflections total and 5480 unique

After rejection, 23934 reflections total and 5475 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0623   0.902 - 1.020   0.950 - 1.103   1.173   21460   13433
    2   -6.8  0.0681   0.637 - 0.760   0.958 - 1.083   1.187    2474    1402
Ratio of minimum to maximum apparent transmission: 0.861147


  Group    Mike Hursthouse  
  Operator   Mike Hursthouse  
  Sample Owner     
  Local Code   TLT374cAB3-4  
  Crystal Colour    Colourless  
  Crystal Habit    Rod  
  Crystal Size   0.12 x 0.03 x 0.03 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   85 (mA) 
  Primary Solvent     
  Other Solvents     

File Explanations

      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

'COLLECT (Hooft, R.W.W., 1998)'
'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
'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. SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10

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/