EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: home/diska/2005src1626

Report generated Dec 12, 2005; 16:19:42

Unit cell

8454 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
c2
a (Angstrom)42.3473 +/- 0.0011
b (Angstrom)9.8261 +/- 0.0003
c (Angstrom)17.1615 +/- 0.0003
alpha (°) 90.000
beta (°)99.7937 +/- 0.0013
gamma (°) 90.000
Volume (A**3)7037.0 +/- 0.3
Mosaicity (°)0.5970 +/- 0.0010

Data collection

Summary

Total number of images collected357
Total exposure time72.1 minutes
Data collection exposure time71.0 minutes
Data collection wall-clock time101.5 minutes

Experimental Conditions

Wavelength0.71073 A
Cryostat setting120.00K
Crystal to detector distance44.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f168252.0° phi1.500°12 secondsYes
data collections02f46 69.0° omega1.500°12 secondsYes
data collections03f90135.0° omega1.500°12 secondsYes
data collections04f45 67.5° omega1.500°12 secondsYes
Phi/Chii01f - i08f88 seconds

Scalepack Scaling

Deleted observations

Rejected 255
Zero sigma or profile test   8
Overload or incomplete profile1546
Sigma cutoff  16
High resolution limit  18

Final Data Set

Scale factor range4.56-10.68
Number of 'full' reflections 20421
Number of 'partial' reflections 21983
Total number of integrated reflections 40531
Total number of unique reflections  8535
Data completeness 100.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   66.1
Average Sigma(I)    2.6
Overall R-merge (linear)  0.065

Sadabs Results

Parameter refinement on 27843 reflections reduced R(int) from 0.0969 to 0.0519

Before rejection, 40495 reflections total and 8546 unique

After rejection, 39958 reflections total and 8545 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   18.3  0.0562   0.608 - 0.880   0.911 - 1.112   1.339   19016   14259
    2  -17.7  0.0796   1.209 - 1.440   0.909 - 1.053   1.410    5259    3273
    3  -17.7  0.0550   0.833 - 1.244   0.909 - 1.046   1.343   10584    7846
    4  -17.7  0.0714   1.245 - 1.730   0.907 - 1.037   1.384    5099    3333
Ratio of minimum to maximum apparent transmission: 0.814947

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. A. Dervisi  
  Local Code   DK191  
  Formula   C32 H29 P1 S1 Cl2 Pd1  
  Crystal Colour    Yellow  
  Crystal Habit    Plate  
  Crystal Size   0.24 x 0.2 x 0.04 (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/