Summary report for Directory: diska/2005src0459r

Report generated Jun 09, 2005; 09:44:43

Unit cell

4037 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) 5.6210 +/- 0.0006

b (Angstrom) 56.453 +/- 0.007

c (Angstrom) 7.8578 +/- 0.0009

alpha (°) 90.000

beta (°) 102.963 +/- 0.005

gamma (°) 90.000

Volume (A**3) 2429.9 +/- 0.5
Mosaicity (°) 0.430 +/- 0.004

Symmetry used in scalepack	p2
a (Angstrom)	5.6210 +/- 0.0006
b (Angstrom)	56.453 +/- 0.007
c (Angstrom)	7.8578 +/- 0.0009
alpha (°)	90.000
beta (°)	102.963 +/- 0.005
gamma (°)	90.000
Volume (A**3)	2429.9 +/- 0.5
Mosaicity (°)	0.430 +/- 0.004

Data collection

Summary

Total number of images collected	546
Total exposure time	13.6 hours
Data collection exposure time	13.5 hours
Data collection wall-clock time	14.6 hours

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	90.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	121	`242.0`° phi	2.000°	90 seconds	Yes
data collection	s02f	148	`296.0`° phi	2.000°	90 seconds	Yes
data collection	s03f	25	`50.0`° omega	2.000°	90 seconds	Yes
data collection	s04f	90	`180.0`° omega	2.000°	90 seconds	Yes
data collection	s05f	40	`80.0`° omega	2.000°	90 seconds	Yes
data collection	s06f	45	`90.0`° omega	2.000°	90 seconds	Yes
data collection	s07f	17	`34.0`° omega	2.000°	90 seconds	Yes
data collection	s08f	52	`104.0`° omega	2.000°	90 seconds	Yes
Phi/Chi	i01f - i08f	8			50 seconds

Scalepack Scaling

Deleted observations

Rejected	`254`
Zero sigma or profile test	`427`
Overload or incomplete profile	`912`
Sigma cutoff	`219`
High resolution limit	`642`

Final Data Set

Scale factor range	0.11-19.77
Number of 'full' reflections	`11854`
Number of 'partial' reflections	`4083`
Total number of integrated reflections	`14909`
Total number of unique reflections	`4790`
Data completeness	`85.0%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`19.3`
Average Sigma(I)	`1.9`
Overall R-merge (linear)	`0.181`

Sadabs Results

Parameter refinement on 8079 reflections reduced R(int) from 0.1632 to 0.0724

Before rejection, 16480 reflections total and 4899 unique

After rejection, 15875 reflections total and 4881 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   -5.2  0.0582   1.810 - 2.618   0.938 - 1.317   1.320    1982    1650
    2   35.0  0.1430   0.490 - 0.833   0.866 - 1.194   1.360    3678    1942
    3  -34.4  0.1532   0.550 - 0.666   0.960 - 1.478   1.479    1293     593
    4  -34.4  0.1212   0.514 - 0.818   0.928 - 1.418   1.311    3173    1696
    5   34.4  0.1078   0.391 - 0.557   0.904 - 1.094   1.295    1184     615
    6   34.2  0.1063   0.513 - 0.703   0.838 - 1.067   1.277     981     436
    7   34.4  0.1528   0.308 - 0.375   0.900 - 1.026   1.292     682     346
    8   34.4  0.1016   0.591 - 1.386   0.922 - 1.113   1.269    2902    1673

Sadabs Results

Parameter refinement on 6752 reflections reduced R(int) from 0.1551 to 0.0673

Before rejection, 13650 reflections total and 4600 unique

After rejection, 13311 reflections total and 4581 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    5.2  0.0644   0.918 - 1.300   0.939 - 1.139   1.449    1698    1355
    2  -35.0  0.1677   0.784 - 1.325   0.932 - 1.162   1.451    2580    1322
    3   34.4  0.1856   0.815 - 1.000   0.904 - 1.157   1.600    1287     580
    4   34.4  0.1326   0.736 - 1.134   0.950 - 1.167   1.387    2598    1415
    5  -34.4  0.1133   0.774 - 1.052   0.926 - 1.127   1.428     757     367
    6  -34.2  0.0785   0.431 - 0.855   0.867 - 1.193   1.239    1137     814
    7  -34.4  0.1568   0.855 - 0.959   0.891 - 1.036   1.388     430     234
    8  -34.4  0.1126   0.427 - 0.957   0.900 - 1.124   1.199    2824    1596

Ratio of minimum to maximum apparent transmission: 0.567015

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. J. H. R. Tucker

Local Code FESCH3

Formula C29 H37 N3 O2 S1 Fe1

Crystal Colour Orange

Crystal Habit Rod

Crystal Size 0.34 x 0.05 x 0.03 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. J. H. R. Tucker
Local Code	FESCH3
Formula	C29 H37 N3 O2 S1 Fe1
Crystal Colour	Orange
Crystal Habit	Rod
Crystal Size	0.34 x 0.05 x 0.03 (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/