EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/04mbh0601

Report generated Jun 17, 2004; 09:51:21

Unit cell

5332 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)7.4044 +/- 0.0002
b (Angstrom)8.2310 +/- 0.0004
c (Angstrom)23.3461 +/- 0.0012
alpha (°)90.8605 +/- 0.0017
beta (°)98.131 +/- 0.003
gamma (°)99.939 +/- 0.003
Volume (A**3)1386.27 +/- 0.11
Mosaicity (°)0.459 +/- 0.002

Data collection


Total number of images collected291
Total exposure time101.4 minutes
Data collection exposure time100.1 minutes
Data collection wall-clock time128.4 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.80 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f259362.6° phi1.400°21 secondsYes
data collections02f24 33.6° omega1.400°21 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 102
Zero sigma or profile test   9
Overload or incomplete profile 488
Sigma cutoff  13
High resolution limit   2

Final Data Set

Scale factor range8.81-10.31
Number of 'full' reflections 10600
Number of 'partial' reflections  8971
Total number of integrated reflections 18690
Total number of unique reflections  6201
Data completeness  97.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   14.7
Average Sigma(I)    1.3
Overall R-merge (linear)  0.062

Sadabs Results

Parameter refinement on 9897 reflections reduced R(int) from 0.0580 to 0.0380

Before rejection, 19094 reflections total and 6225 unique

After rejection, 18909 reflections total and 6223 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.2  0.0602   0.908 - 1.049   0.895 - 1.217   1.152   17441   10714
    2   -7.6  0.0569   0.599 - 0.689   0.916 - 1.101   1.163    1468     883
Ratio of minimum to maximum apparent transmission: 0.735219


  Group    Mike Hursthouse  
  Operator   Mike Hursthouse  
  Sample Owner     
  Local Code   tlt374aAB9/10  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.2 x 0.2 x 0.06 (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/