EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/04src0772

Report generated Sep 30, 2004; 16:56:19

Unit cell

7075 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)8.7627 +/- 0.0003
b (Angstrom)13.8502 +/- 0.0004
c (Angstrom)14.3230 +/- 0.0004
alpha (°)72.574 +/- 0.002
beta (°)75.0895 +/- 0.0017
gamma (°)75.365 +/- 0.002
Volume (A**3)1573.35 +/- 0.09
Mosaicity (°)0.893 +/- 0.002

Data collection

Summary

Total number of images collected305
Total exposure time151.0 minutes
Data collection exposure time149.6 minutes
Data collection wall-clock time178.3 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°30 secondsYes
data collections02f16 32.0° omega2.000°30 secondsYes
data collections03f23 46.0° omega2.000°30 secondsYes
data collections04f23 46.0° omega2.000°30 secondsYes
data collections05f54108.0° omega2.000°30 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected1034
Overload or incomplete profile1392
Sigma cutoff  30
High resolution limit  15

Final Data Set

Scale factor range5.71-12.66
Number of 'full' reflections 13675
Number of 'partial' reflections 20745
Total number of integrated reflections 32727
Total number of unique reflections  7265
Data completeness  98.6%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   96.1
Average Sigma(I)    3.6
Overall R-merge (linear)  0.077

Eval Integration

Data set b-a/final.y

No post-processing summary file exists for this data set

Data set a-b/final.y

Number of reflections 33905
Unique reflections  7837
Weak reflections  6738
Negative intensities   104
R-sym 0.225
R-meas 0.251

Sadabs Results

Parameter refinement on 24968 reflections reduced R(int) from 0.1954 to 0.0770

Before rejection, 32844 reflections total and 7274 unique

After rejection, 31984 reflections total and 7274 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0949   0.736 - 1.494   0.961 - 1.275   1.420   19788   15659
    2   -6.8  0.1106   0.745 - 0.832   0.962 - 1.103   1.407    1530    1279
    3   -6.8  0.1714   0.809 - 1.093   0.965 - 1.267   1.558    2313    1713
    4   -6.8  0.1076   0.683 - 0.765   0.962 - 1.111   1.382    2388    1770
    5   -6.8  0.0888   0.653 - 0.913   0.963 - 1.237   1.344    5965    4946

Sadabs Results

CompareCell Results

{Input cell   : a=8.7496 b=13.8365 c=14.3072 alpha=72.530 beta=75.045 gamma=75.284 P
 Reduced cell : a=8.7496 b=13.8365 c=14.3072 alpha=72.530 beta=75.045 gamma=75.284
 Transformed  : a=8.7496 b=13.8365 c=14.3072 alpha=72.530 beta=75.045 gamma=75.284 P
 Volume       : 1566.65; System: triclinic; Point group: -1}
{Input cell   : a=8.7459 b=13.8251 c=14.2934 alpha=72.599 beta=75.049 gamma=75.330 P
 Reduced cell : a=8.7459 b=13.8251 c=14.2934 alpha=72.599 beta=75.049 gamma=75.330
 Transformed  : a=8.7459 b=13.8251 c=14.2934 alpha=72.599 beta=75.049 gamma=75.330 P
 Volume       : 1564.00; System: triclinic; Point group: -1}
==============================================================================
Solution number :   1
---------------------
New Cell: a=8.7459 b=13.8251 c=14.2934 alpha=72.599 beta=75.049 gamma=75.330

Figure of Merit (0=ideal)         :   0.51
Rotation angle  (degrees)         : 179.999
Rotation vector (laboratory)      :  -0.6692  0.7034  0.2396
Rotation vector (reciprocal cell) :  -2.00   -1.01   -1.01
Rotation vector (direct cell)     :  -1.00   -0.04   -0.02

Superposition matrix              : H' = +0.937 * H +0.076 * K +0.047 * L
                                    K' = +0.978 * H -0.961 * K +0.024 * L
                                    L' = +0.977 * H +0.039 * K -0.975 * L
==============================================================================

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Lancaster  
  Local Code   DP3-56  
  Formula   C21H26NO2Cl3Zr  
  Crystal Colour    Yellow  
  Crystal Habit    Rod  
  Crystal Size   0.18 x 0.04 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/