Summary report for Directory: diska/05src0055

Report generated Jan 20, 2005; 16:45:28

Unit cell

3480 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack p222

a (Angstrom) 12.9280 +/- 0.0003

b (Angstrom) 14.1449 +/- 0.0003

c (Angstrom) 14.7823 +/- 0.0002

alpha (°) 90.000

beta (°) 90.000

gamma (°) 90.000

Volume (A**3) 2703.17 +/- 0.09
Mosaicity (°) 0.3570 +/- 0.0010

Symmetry used in scalepack	p222
a (Angstrom)	12.9280 +/- 0.0003
b (Angstrom)	14.1449 +/- 0.0003
c (Angstrom)	14.7823 +/- 0.0002
alpha (°)	90.000
beta (°)	90.000
gamma (°)	90.000
Volume (A**3)	2703.17 +/- 0.09
Mosaicity (°)	0.3570 +/- 0.0010

Data collection

Summary

Total number of images collected	197
Total exposure time	52.4 minutes
Data collection exposure time	51.1 minutes
Data collection wall-clock time	68.2 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	35.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	117	`234.0`° phi	2.000°	16 seconds	Yes
data collection	s02f	16	`32.0`° omega	2.000°	16 seconds	Yes
data collection	s03f	56	`112.0`° omega	2.000°	16 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`151`
Zero sigma or profile test	`5`
Overload or incomplete profile	`906`
Sigma cutoff	`5`
High resolution limit	`33`

Final Data Set

Scale factor range	9.14-10.06
Number of 'full' reflections	`22701`
Number of 'partial' reflections	`8094`
Total number of integrated reflections	`29553`
Total number of unique reflections	`3487`
Data completeness	`100.0%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`72.0`
Average Sigma(I)	`1.6`
Overall R-merge (linear)	`0.035`

Sadabs Results

Parameter refinement on 21642 reflections reduced R(int) from 0.0554 to 0.0324

Before rejection, 29468 reflections total and 3496 unique

After rejection, 29229 reflections total and 3496 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0349   0.966 - 1.046   0.950 - 1.092   1.282   18332   13890
    2  -11.2  0.0316   0.754 - 0.788   0.953 - 1.041   1.198    2239    1695
    3  -11.2  0.0364   0.910 - 0.959   0.959 - 1.052   1.297    8658    6602

Ratio of minimum to maximum apparent transmission: 0.869914

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. P. J. Skabara

Local Code BisEDTT

Formula C12 H10 S6

Crystal Colour Colourless

Crystal Habit Cut Block

Crystal Size 0.38 x 0.25 x 0.15 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. P. J. Skabara
Local Code	BisEDTT
Formula	C12 H10 S6
Crystal Colour	Colourless
Crystal Habit	Cut Block
Crystal Size	0.38 x 0.25 x 0.15 (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/