EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2006slh0985

Report generated Oct 16, 2006; 15:07:20

Unit cell

4888 reflections with 1.00°<theta<27.48° (resolution between 20.40A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p1
a (Angstrom)9.1961 +/- 0.0003
b (Angstrom)10.5439 +/- 0.0004
c (Angstrom)12.5033 +/- 0.0004
alpha (°)113.9482 +/- 0.0017
beta (°)98.202 +/- 0.002
gamma (°)95.732 +/- 0.002
Volume (A**3)1079.84 +/- 0.07
Mosaicity (°)0.499 +/- 0.002

Data collection

Summary

Total number of images collected325
Total exposure time265.3 minutes
Data collection exposure time263.6 minutes
Data collection wall-clock time5.6 hours

Experimental Conditions

Wavelength0.71073 A

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Detector
distance		Used in
scaling
cell determinationi01f10 10.0° phi1.000°10 seconds45.00 mmNo
data collections01f181362.0° phi2.000°50 seconds30.00 mmYes
data collections02f17 34.0° omega2.000°50 seconds30.00 mmYes
data collections03f16 32.0° omega2.000°50 seconds30.00 mmYes
data collections04f23 46.0° omega2.000°50 seconds30.00 mmYes
data collections05f55110.0° omega2.000°50 seconds30.00 mmYes
data collections06f23 46.0° omega2.000°50 seconds30.00 mmYes

Scalepack Scaling

Deleted observations

Rejected 112
Zero sigma or profile test   3
Overload or incomplete profile 554
Sigma cutoff  36
High resolution limit  45

Final Data Set

Scale factor range9.90-10.46
Number of 'full' reflections 16221
Number of 'partial' reflections  9143
Total number of integrated reflections 24442
Total number of unique reflections  4936
Data completeness  99.9%
Resolution range20.40-0.77 A
Theta range1.00°-27.48°
Average Intensity   23.8
Average Sigma(I)    1.3
Overall R-merge (linear)  0.059

Sadabs Results

Parameter refinement on 14754 reflections reduced R(int) from 0.0599 to 0.0422

Before rejection, 24000 reflections total and 4960 unique

After rejection, 23772 reflections total and 4956 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0597   1.031 - 1.169   0.981 - 1.151   1.145   13955    9569
    2   -6.8  0.0548   0.618 - 0.654   0.986 - 1.082   1.175    1172     777
    3   -6.8  0.0573   0.588 - 0.626   0.984 - 1.095   1.072    1104     767
    4   -6.8  0.0572   0.543 - 0.572   0.986 - 1.129   1.144    1651    1140
    5   -6.8  0.0626   0.968 - 1.082   0.985 - 1.122   1.105    4223    2886
    6   -6.8  0.0576   1.054 - 1.094   0.986 - 1.112   1.095    1667    1164
Ratio of minimum to maximum apparent transmission: 0.853041

Metadata

  Group    Personal  
  Operator   Susanne Huth  
  Sample Owner   Cagliari  
  Local Code   CAG 172  
  Formula   C44 H48 N2 O4 P2 S4 Fe1 Ni1  
  Crystal Colour    Light Brown  
  Crystal Habit    Block  
  Crystal Size   0.24 x 0.08 x 0.06 (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    '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

_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/