EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2005src0655r

Report generated Jun 23, 2005; 16:52:45

Unit cell

a (Angstrom)15.243 +/- 0.004
b (Angstrom)32.288 +/- 0.003
c (Angstrom)32.342 +/- 0.012
alpha (°)90.089 +/- 0.018
beta (°)90.21 +/- 0.02
gamma (°)90.010 +/- 0.011
Volume (A**3)15918. +/- 6.

Data collection

Summary

Total number of images collected615
Total exposure time12.2 hours
Data collection exposure time12.2 hours
Data collection wall-clock time13.1 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance75.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame
data collections01f223267.6° phi1.200°72 seconds
data collections02f198237.6° phi1.200°72 seconds
data collections03f51 61.2° omega1.200°72 seconds
data collections04f70 84.0° omega1.200°72 seconds
data collections05f65 78.0° omega1.200°72 seconds
Phi/Chii01f - i08f830 seconds

Sadabs Results

Parameter refinement on 102676 reflections reduced R(int) from 0.4516 to 0.0785

Before rejection, 128278 reflections total and 36184 unique

After rejection, 82208 reflections total and 31430 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1  -16.0  0.0527   0.955 - 1.218   0.936 - 1.323   1.765   19382   18744
    2   31.3  0.0773   0.699 - 0.867   0.875 - 1.160   1.887   31368   22952
    3  -30.8  0.0730   0.846 - 0.914   0.977 - 1.530   1.803    8240    6272
    4  -30.8  0.0616   0.994 - 1.117   0.916 - 1.630   1.814   12637    9786
    5   30.8  0.0744   0.795 - 0.957   0.920 - 1.087   1.812   10581    8158

Sadabs Results

Parameter refinement on 81351 reflections reduced R(int) from 0.4141 to 0.0718

Before rejection, 103728 reflections total and 30190 unique

After rejection, 66262 reflections total and 26291 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   16.0  0.0467   0.785 - 0.992   0.941 - 1.361   1.726   19126   18050
    2  -31.3  0.0633   0.816 - 1.084   0.913 - 1.140   1.887   24370   17648
    3   30.8  0.0531   0.830 - 0.922   1.003 - 1.475   1.786    6177    4549
    4   30.8  0.0516   0.823 - 0.937   0.928 - 1.691   1.796    9259    7108
    5  -30.8  0.0632   0.920 - 1.116   0.840 - 1.107   1.928    7330    5825
Ratio of minimum to maximum apparent transmission: 0.537139

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. A. Dervisi  
  Local Code   SB269  
  Formula   C58 H48 P2 S2 Cl2 Pd2  
  Crystal Colour    Red  
  Crystal Habit   Cut Block  
  Crystal Size   0.28 x 0.26 x 0.18 (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/