EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2005src1621

Report generated Jan 19, 2006; 08:41:41

Unit cell

36779 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)13.6780 +/- 0.0005
b (Angstrom)16.2313 +/- 0.0006
c (Angstrom)42.7653 +/- 0.0015
alpha (°)96.1577 +/- 0.0014
beta (°)91.7587 +/- 0.0014
gamma (°)106.9006 +/- 0.0009
Volume (A**3)9012.8 +/- 0.6
Mosaicity (°)0.4520 +/- 0.0010

Data collection

Summary

Total number of images collected822
Total exposure time13.7 hours
Data collection exposure time13.6 hours
Data collection wall-clock time14.7 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance65.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f242363.0° phi1.500°60 secondsYes
data collections02f115172.5° omega1.500°60 secondsYes
data collections03f41 61.5° omega1.500°60 secondsYes
data collections04f40 60.0° omega1.500°60 secondsYes
data collections05f40 60.0° omega1.500°60 secondsYes
data collections06f68102.0° omega1.500°60 secondsYes
data collections07f48 72.0° omega1.500°60 secondsYes
data collections08f48 72.0° omega1.500°60 secondsYes
data collections09f37 55.5° omega1.500°60 secondsYes
data collections10f74111.0° omega1.500°60 secondsNo
data collections11f61 91.5° omega1.500°60 secondsNo
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected4995
Zero sigma or profile test 583
Overload or incomplete profile4060
Sigma cutoff 373
Low resolution limit  16
High resolution limit5559

Final Data Set

Scale factor range0.14-17.82
Number of 'full' reflections 81550
Number of 'partial' reflections 47606
Total number of integrated reflections120666
Total number of unique reflections 39413
Data completeness  94.6%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   29.4
Average Sigma(I)    3.4
Overall R-merge (linear)  0.334

Sadabs Results

Parameter refinement on 72636 reflections reduced R(int) from 0.3067 to 0.0627

Before rejection, 160820 reflections total and 41826 unique

After rejection, 147428 reflections total and 41061 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   28.2  0.0963   0.770 - 1.458   0.916 - 1.233   1.381   47472   24297
    2  -27.6  0.0921   0.837 - 1.029   0.925 - 1.160   1.351   23339   12426
    3  -27.6  0.0924   0.614 - 0.916   0.922 - 1.092   1.382    8048    4611
    4  -27.6  0.0803   0.473 - 0.872   0.902 - 1.122   1.353    6350    3685
    5  -27.6  0.3872   0.670 - 1.037   0.990 - 1.271   1.858    4469    1192
    6  -27.6  0.0737   0.842 - 1.251   0.899 - 1.133   1.346   10164    6070
    7  -27.6  0.7373   0.771 - 1.178   0.984 - 1.279   1.901    5678     694
    8  -27.6  0.0903   0.659 - 0.873   0.914 - 1.091   1.368    9467    5207
    9  -27.6  0.2257   0.698 - 0.989   0.923 - 1.163   1.702    6127    2030
   10  -27.6  0.1103   0.620 - 0.998   0.909 - 1.126   1.405   14163    7206
   11  -27.6  0.0986   0.576 - 1.024   0.929 - 1.130   1.376   12151    6723
Ratio of minimum to maximum apparent transmission: 0.702517

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Prof. M. Bochmann  
  Local Code   RH356  
  Formula   C60 H70 N2 O4 Ti1  
  Crystal Colour    Yellow  
  Crystal Habit    Lath  
  Crystal Size   0.36 x 0.06 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 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/