EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/04mbh0603

Report generated Jun 18, 2004; 08:57:22

Unit cell

2051 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)20.0660 +/- 0.0010
b (Angstrom)7.6117 +/- 0.0002
c (Angstrom)15.2613 +/- 0.0008
alpha (°) 90.000
beta (°)129.9326 +/- 0.0014
gamma (°) 90.000
Volume (A**3)1787.38 +/- 0.14
Mosaicity (°)0.460 +/- 0.002

Data collection


Total number of images collected175
Total exposure time57.6 minutes
Data collection exposure time56.3 minutes
Data collection wall-clock time70.7 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.80 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f152304.0° phi2.000°20 secondsYes
data collections02f15 30.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 126
Zero sigma or profile test   1
Overload or incomplete profile 378
Sigma cutoff  12

Final Data Set

Scale factor range9.03-12.57
Number of 'full' reflections  7139
Number of 'partial' reflections  3474
Total number of integrated reflections 10283
Total number of unique reflections  2203
Data completeness  99.1%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   72.6
Average Sigma(I)    2.4
Overall R-merge (linear)  0.070

Sadabs Results

Parameter refinement on 7142 reflections reduced R(int) from 0.1363 to 0.0544

Before rejection, 10228 reflections total and 2202 unique

After rejection, 10029 reflections total and 2201 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.2  0.0589   0.762 - 1.167   0.936 - 1.134   1.393    9201    6699
    2   -7.6  0.0623   0.482 - 0.557   0.943 - 1.084   1.381     828     608
Ratio of minimum to maximum apparent transmission: 0.825756


  Group    Mike Hursthouse  
  Operator   Mike Hursthouse  
  Sample Owner     
  Local Code   TLT374aGH1-2  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.1 x 0.1 x 0.05 (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    '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

'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/