EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2010src0043

Report generated Feb 12, 2010; 16:30:58

Unit cell

77283 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p1
a (Angstrom)10.0905 +/- 0.0002
b (Angstrom)12.7583 +/- 0.0004
c (Angstrom)14.4492 +/- 0.0005
alpha (°)100.0257 +/- 0.0015
beta (°)98.125 +/- 0.002
gamma (°)108.201 +/- 0.002
Volume (A**3)1701.60 +/- 0.09
Mosaicity (°)1.356 +/- 0.002

Data collection

Summary

Total number of images collected452
Total exposure time136.7 minutes
Data collection exposure time135.6 minutes
Data collection wall-clock time160.7 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance31.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f242363.0° phi1.500°18 secondsYes
data collections02f18 27.0° omega1.500°18 secondsYes
data collections03f32 48.0° omega1.500°18 secondsYes
data collections04f32 48.0° omega1.500°18 secondsYes
data collections05f42 63.0° omega1.500°18 secondsYes
data collections06f25 37.5° omega1.500°18 secondsYes
data collections07f21 31.5° omega1.500°18 secondsYes
data collections08f32 48.0° omega1.500°18 secondsYes
Phi/Chii01f - i08f88 seconds

Scalepack Scaling

Deleted observations

Rejected   4
Zero sigma or profile test   3
Overload or incomplete profile1588
Sigma cutoff 703
High resolution limit 181

Final Data Set

Scale factor10.00
Number of 'full' reflections   925
Number of 'partial' reflections 35148
Total number of integrated reflections 32480
Total number of unique reflections  7736
Data completeness  99.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  100.3
Average Sigma(I)    3.2
Overall R-merge (linear)  0.242

Sadabs Results

Parameter refinement on 27276 reflections reduced R(int) from 0.1425 to 0.0770

Before rejection, 32721 reflections total and 7804 unique

After rejection, 29021 reflections total and 7756 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.7  0.0603   0.737 - 1.298   0.925 - 1.218   2.035   16802   14513
    2   11.1  0.0859   0.741 - 0.801   0.947 - 1.130   2.172    1019     839
    3   11.1  0.2056   0.994 - 1.291   0.927 - 1.179   2.424    1804    1167
    4   11.1  0.1291   0.854 - 1.510   0.947 - 1.130   2.384    1799    1267
    5   11.1  0.0565   0.731 - 0.837   0.926 - 1.126   2.076    2819    2507
    6   11.1  0.0554   0.645 - 0.691   0.947 - 1.131   2.057    1559    1350
    7   11.1  0.0588   0.685 - 0.733   0.971 - 1.140   1.921    1272    1104
    8   11.1  0.0934   0.586 - 0.848   0.947 - 1.138   2.305    1947    1429
Ratio of minimum to maximum apparent transmission: 0.759411

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr SL James  
  Local Code   CD67  
  Formula   C40 H38 P2 Pt Cl2  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Blade  
  Crystal Size   0.08 x 0.05 x 0.02 (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 2007/2 (Sheldrick, G.M., 2007)'

_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 APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

_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. (2007). SADABS. Version 2007/2. 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/