Summary report for Directory: diska/04src0949_295

Report generated Dec 09, 2004; 14:35:44

Unit cell

2220 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) 7.3692 +/- 0.0004

b (Angstrom) 7.3843 +/- 0.0004

c (Angstrom) 17.0158 +/- 0.0007

alpha (°) 90.032

beta (°) 89.988

gamma (°) 120.086

Volume (A**3) 801.19 +/- 0.07
Mosaicity (°) 0.378 +/- 0.004

Symmetry used in scalepack	p1
a (Angstrom)	7.3692 +/- 0.0004
b (Angstrom)	7.3843 +/- 0.0004
c (Angstrom)	17.0158 +/- 0.0007
alpha (°)	90.032
beta (°)	89.988
gamma (°)	120.086
Volume (A**3)	801.19 +/- 0.07
Mosaicity (°)	0.378 +/- 0.004

Data collection

Summary

Total number of images collected	134
Total exposure time	85.8 minutes
Data collection exposure time	84.4 minutes
Data collection wall-clock time	96.1 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	30.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	80	`160.0`° phi	2.000°	40 seconds	Yes
data collection	s02f	22	`44.0`° omega	2.000°	40 seconds	Yes
data collection	s03f	24	`48.0`° omega	2.000°	40 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`13`
Overload or incomplete profile	`188`
Sigma cutoff	`4`
High resolution limit	`7`

Final Data Set

Scale factor range	9.48-10.00
Number of 'full' reflections	`5387`
Number of 'partial' reflections	`2112`
Total number of integrated reflections	`6885`
Total number of unique reflections	`3330`
Data completeness	`90.5%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`95.9`
Average Sigma(I)	`3.9`
Overall R-merge (linear)	`0.023`

Sadabs Results

Parameter refinement on 1797 reflections reduced R(int) from 0.0775 to 0.0202

Before rejection, 7052 reflections total and 3374 unique

After rejection, 6992 reflections total and 3371 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0229   0.928 - 1.000   0.836 - 1.136   1.242    4578    1430
    2   -6.8  0.0214   0.991 - 1.048   0.924 - 1.047   1.157    1149     374
    3   -6.8  0.0239   0.944 - 1.037   0.965 - 1.039   1.242    1265     406

Ratio of minimum to maximum apparent transmission: 0.736088

Metadata

Group Service

Operator Simon Coles

Sample Owner Wills

Local Code H3OFe(24)

Formula Fe3S2O15H9

Crystal Colour Orange

Crystal Habit Block

Crystal Size 0.08 x 0.08 x 0.08 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Simon Coles
Sample Owner	Wills
Local Code	H3OFe(24)
Formula	Fe3S2O15H9
Crystal Colour	Orange
Crystal Habit	Block
Crystal Size	0.08 x 0.08 x 0.08 (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/