Summary report for Directory: diska/04src0951_295

Report generated Dec 15, 2004; 08:56:06

Unit cell

2351 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) 7.3042 +/- 0.0004

b (Angstrom) 7.3048 +/- 0.0005

c (Angstrom) 17.2256 +/- 0.0015

alpha (°) 89.984 +/- 0.004

beta (°) 89.995 +/- 0.005

gamma (°) 119.996 +/- 0.004

Volume (A**3) 795.98 +/- 0.10
Mosaicity (°) 0.345 +/- 0.004

Symmetry used in scalepack	p1
a (Angstrom)	7.3042 +/- 0.0004
b (Angstrom)	7.3048 +/- 0.0005
c (Angstrom)	17.2256 +/- 0.0015
alpha (°)	89.984 +/- 0.004
beta (°)	89.995 +/- 0.005
gamma (°)	119.996 +/- 0.004
Volume (A**3)	795.98 +/- 0.10
Mosaicity (°)	0.345 +/- 0.004

Data collection

Summary

Total number of images collected	126
Total exposure time	5.3 hours
Data collection exposure time	5.3 hours
Data collection wall-clock time	5.6 hours

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	69	`138.0`° phi	2.000°	160 seconds	Yes
data collection	s02f	49	`98.0`° omega	2.000°	160 seconds	Yes
Phi/Chi	i01f - i08f	8			40 seconds

Scalepack Scaling

Deleted observations

Rejected	`27`
Zero sigma or profile test	`1`
Overload or incomplete profile	`164`
Sigma cutoff	`5`
High resolution limit	`4`

Final Data Set

Scale factor range	9.65-10.00
Number of 'full' reflections	`5293`
Number of 'partial' reflections	`1724`
Total number of integrated reflections	`6842`
Total number of unique reflections	`3367`
Data completeness	`91.8%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`55.0`
Average Sigma(I)	`3.0`
Overall R-merge (linear)	`0.033`

Sadabs Results

Parameter refinement on 1652 reflections reduced R(int) from 0.0388 to 0.0222

Before rejection, 6709 reflections total and 3369 unique

After rejection, 6618 reflections total and 3361 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0294   0.928 - 1.035   0.888 - 1.195   1.248    3872    1235
    2    6.9  0.0307   0.924 - 1.001   0.917 - 1.189   1.291    2746     873

Ratio of minimum to maximum apparent transmission: 0.742873

Metadata

Group Service

Operator Simon Coles

Sample Owner Wills

Local Code KFe

Formula KFe3S2O14H6

Crystal Colour Orange

Crystal Habit Block

Crystal Size 0.05 x 0.05 x 0.05 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Simon Coles
Sample Owner	Wills
Local Code	KFe
Formula	KFe3S2O14H6
Crystal Colour	Orange
Crystal Habit	Block
Crystal Size	0.05 x 0.05 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    '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/