Summary report for Directory: home/diska/04src0821

Report generated Sep 23, 2004; 11:12:21

Unit cell

1590 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack p2

a (Angstrom) 7.8223 +/- 0.0008

b (Angstrom) 24.143 +/- 0.003

c (Angstrom) 7.9681 +/- 0.0009

alpha (°) 90.000

beta (°) 118.611 +/- 0.006

gamma (°) 90.000

Volume (A**3) 1321.1 +/- 0.3
Mosaicity (°) 1.649 +/- 0.003

Symmetry used in scalepack	p2
a (Angstrom)	7.8223 +/- 0.0008
b (Angstrom)	24.143 +/- 0.003
c (Angstrom)	7.9681 +/- 0.0009
alpha (°)	90.000
beta (°)	118.611 +/- 0.006
gamma (°)	90.000
Volume (A**3)	1321.1 +/- 0.3
Mosaicity (°)	1.649 +/- 0.003

Data collection

Summary

Total number of images collected	389
Total exposure time	78.9 minutes
Data collection exposure time	77.5 minutes
Data collection wall-clock time	108.9 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	40.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	262	`262.0`° phi	1.000°	12 seconds	Yes
data collection	s02f	63	`63.0`° omega	1.000°	12 seconds	Yes
data collection	s03f	56	`56.0`° omega	1.000°	12 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`442`
Zero sigma or profile test	`13`
Overload or incomplete profile	`722`
Sigma cutoff	`19`
Low resolution limit	`14`
High resolution limit	`3`

Final Data Set

Scale factor range	10.00-68.31
Number of 'full' reflections	`0`
Number of 'partial' reflections	`9127`
Total number of integrated reflections	`6217`
Total number of unique reflections	`2518`
Data completeness	`79.3%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`34.8`
Average Sigma(I)	`2.3`
Overall R-merge (linear)	`0.079`

Sadabs Results

Parameter refinement on 7263 reflections reduced R(int) from 0.2656 to 0.0845

Before rejection, 11687 reflections total and 3106 unique

After rejection, 10682 reflections total and 3100 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.6  0.0957   0.585 - 1.470   0.754 - 1.903   1.472    7377    4468
    2  -15.0  0.0926   0.577 - 0.748   0.728 - 2.458   1.603    1677    1108
    3  -15.0  0.0578   0.712 - 0.813   0.826 - 2.755   1.274    1628    1340

Ratio of minimum to maximum apparent transmission: 0.264178

Metadata

Group Service

Operator Simon Coles

Sample Owner Skabara

Local Code HJ EDTT Butyl

Formula C10H12Br2S3

Crystal Colour Colourless

Crystal Habit Slab

Crystal Size 0.38 x 0.14 x 0.05 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Simon Coles
Sample Owner	Skabara
Local Code	HJ EDTT Butyl
Formula	C10H12Br2S3
Crystal Colour	Colourless
Crystal Habit	Slab
Crystal Size	0.38 x 0.14 x 0.05 (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/