Summary report for Directory: diska/04src0333

Report generated May 06, 2004; 09:08:18

Unit cell

244394 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) 14.6900 +/- 0.0005

b (Angstrom) 19.6829 +/- 0.0007

c (Angstrom) 25.4940 +/- 0.0008

alpha (°) 90.000

beta (°) 93.8185 +/- 0.0013

gamma (°) 90.000

Volume (A**3) 7355.0 +/- 0.4
Mosaicity (°) 1.3960 +/- 0.0010

Symmetry used in scalepack	p2
a (Angstrom)	14.6900 +/- 0.0005
b (Angstrom)	19.6829 +/- 0.0007
c (Angstrom)	25.4940 +/- 0.0008
alpha (°)	90.000
beta (°)	93.8185 +/- 0.0013
gamma (°)	90.000
Volume (A**3)	7355.0 +/- 0.4
Mosaicity (°)	1.3960 +/- 0.0010

Data collection

Summary

Total number of images collected	755
Total exposure time	14.6 hours
Data collection exposure time	14.6 hours
Data collection wall-clock time	15.8 hours

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	50.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	143	`143.0`° omega	1.000°	70 seconds	Yes
data collection	s02f	151	`151.0`° omega	1.000°	70 seconds	Yes
data collection	s03f	151	`151.0`° omega	1.000°	70 seconds	Yes
data collection	s04f	151	`151.0`° omega	1.000°	70 seconds	Yes
data collection	s05f	151	`151.0`° omega	1.000°	70 seconds	Yes
Phi/Chi	i01f - i08f	8			30 seconds

Scalepack Scaling

Deleted observations

Rejected	`55`
Zero sigma or profile test	`135`
Overload or incomplete profile	`5650`
Sigma cutoff	`170`
High resolution limit	`725`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`0`
Number of 'partial' reflections	`103992`
Total number of integrated reflections	`96491`
Total number of unique reflections	`17073`
Data completeness	`99.1%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`36.2`
Average Sigma(I)	`2.1`
Overall R-merge (linear)	`0.073`

Sadabs Results

Parameter refinement on 61039 reflections reduced R(int) from 0.0583 to 0.0403

Before rejection, 103257 reflections total and 17368 unique

After rejection, 102552 reflections total and 17368 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1  -13.3  0.0569   0.734 - 0.822   0.958 - 1.257   1.383   17790   12472
    2  -21.1  0.0666   0.777 - 0.914   0.923 - 1.164   1.243   21167   13254
    3  -21.1  0.0647   1.293 - 1.533   0.890 - 1.073   1.231   21176   13342
    4  -21.1  0.0664   1.227 - 1.601   0.925 - 1.305   1.243   21238   13203
    5  -21.1  0.0648   0.693 - 0.749   0.890 - 1.078   1.239   21181   13483

Ratio of minimum to maximum apparent transmission: 0.681895

Metadata

Supervisor Service

Operator Peter Horton

Sample Owner Craig Matthews

Local Code LJD361Fe

Formula C72 H66 N36 O32 Cl8 Fe4

Crystal Colour Dark Brown

Crystal Habit Block

Crystal Size 0.28 x 0.12 x 0.08 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Supervisor	Service
Operator	Peter Horton
Sample Owner	Craig Matthews
Local Code	LJD361Fe
Formula	C72 H66 N36 O32 Cl8 Fe4
Crystal Colour	Dark Brown
Crystal Habit	Block
Crystal Size	0.28 x 0.12 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, 1998)'
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 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, 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. SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10

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/